Quantum printing nanostructures within carbon nanopores

ABSTRACT

The invention includes apparatus and methods for instantiating and quantum printing materials, such as elemental metals, in a nanoporous carbon powder.

RELATED APPLICATIONS

This application is a continuation of U.S. application Ser. No.17/408,821, filed Aug. 23, 2021, which is a continuation of U.S.application Ser. No. 17/122,355, filed Dec. 15, 2020, which is relatedto and claims the benefit of priority under 35 USC 119(e) to provisionalapplication U.S. Ser. No. 62/948,450, by Christopher J. Nagel, filed onDec. 16, 2019. The entire teachings of the above applications areincorporated herein by reference.

BACKGROUND OF THE INVENTION

The detection of metals and other elements in materials subjected toharmonic electromagnetic fields in metal baths and other environmentshas been documented. See, for example, U.S. Pat. Nos. 7,238,297 and9,790,574 to Christopher Nagel, which are incorporated herein byreference.

The present invention relates to the discovery that carbon matrices canbe used to produce nano-deposits, nanostructures, nanowires and nuggetscomprising metals using the processes described herein. The processes ofthe invention include the application of electromagnetic radiation,directly and/or indirectly, to gases, nano-porous carbon, orcompositions and combinations thereof, thereby pre-treating the gas, andexposing a carbon matrix to pre-treated gas in an apparatus of theinvention to cause metal instantiation, nucleation, growth and/ordeposition within the carbon matrix.

SUMMARY OF THE INVENTION

The invention relates to methods of quantum printing and/orinstantiating materials, such as metals (e.g., copper, platinum,platinum group metal (PGMs) or precious metals), in nanoporous carbonmatrices to form nanowires and other macrostructures, and apparatusesadapted for the methods.

The invention includes processes comprising the steps of contacting abed comprising nanoporous carbon with an activated gas while applyingelectromagnetic radiation to the nanoporous carbon for a time sufficientto cause instantiation, including but not limited to nucleation, growthdeposition and/or agglomeration, of elemental metal nanoparticles withinand/or from carbon nanopores and nano-pore networks and matrices. Theprocess results in nanoporous carbon compositions or matricescharacterized by elemental metals deposited within carbon nanopores andagglomerated elemental nanoparticles, creating elemental metal nuggets,nanowires and other macrostructures that can be easily separated fromthe nanoporous carbon.

The processes of the invention have broad applicability in producingelemental metal composition and macrostructures. The invention furtherrelates to the nanoporous carbon compositions, elemental metalnanoparticles and elemental macrostructures produced by the methods ofthe invention.

The invention further relates to elemental macrostructures and elementalmicrostructures harvested from such carbon compositions. For example,the invention includes platinum and platinum group metal compositions.The compositions typically comprise internal carbon.

More specifically, the invention includes a process of quantum printinga metal, such as copper, within a nanoporous carbon powder comprisingthe steps of:

(i) adding a nanoporous carbon powder into a reactor assembly (RA), asdescribed below,

(ii) adding a gas free of metal salts and vaporized metals to thereactor assembly;

(iii) powering the one or more RA coils to a first electromagneticenergy level;

(iv) subjecting the nanoporous carbon powder to harmonic patterning todeposit elemental metal (e.g., copper) nanostructures.

The process contemplates one or more RA frequency generators in RA coilssurrounding a nanoporous carbon bed to establish a harmonicelectromagnetic resonance in ultramicropores of the nanoporous carbonpowder. The gas can be, for example, air, oxygen, hydrogen, helium,nitrogen, neon, argon, krypton, xenon, carbon monoxide, carbon dioxideor mixtures thereof. Preferably, the nanoporous carbon powder comprisesgraphene having at least 99.9% wt. carbon (metals basis), a mass meandiameter between 1 μm and 5 mm, and an ultramicropore surface areabetween about 100 and 3000 m²/g.

The process deposits metal (e.g., copper) atoms in a plurality ofdiscrete rows on the nanoporous carbon powder, thereby forming acarbon-metal interface, which can be sp² carbon. The orderednano-deposit array can comprise discrete rows of nano-deposits, whereinthe nano-deposits are characterized by a diameter of between about 0.1and 0.3 nm, and the space between copper deposit rows is less than about1 nm. The ordered nano-deposit array can be characterized by a carbonrich area and a copper rich area adjacent to the array and the discreterows can be spaced to form a gradient.

More specifically, the invention includes a reactor assembly comprising:

-   -   (a) A reactor chamber containing a nanoporous carbon material;    -   (b) A second porous frit defining the ceiling of the reactor        chamber; wherein each porous frit has a porosity that is        sufficient to allow a gas to permeate into the reactor chamber        and contain a nanoporous carbon material;    -   (c) A reactor head space disposed above the reactor cap;    -   (d) 2, 3, 4, 5 or more (preferably 5) RA coils surrounding the        reactor chamber and/or reactor head space operably connected to        one or more RA frequency generators and one or more power        supplies;    -   (e) 2, 3, 4, 5 or more pairs of RA lamps wherein the pairs of RA        lamps are disposed circumferentially around the RA coils and        define a space between the pairs of RA lamps and the RA coils;    -   (f) An x-ray source configured to expose the reactor chamber to        x-rays;    -   (g) One or more lasers configured to direct a laser towards        (e.g., through or across) the reactor chamber or the gas within        the reactor assembly; and    -   (h) A computer processing unit (CPU) configured to control the        power supply, frequency generator, x-ray source and one or more        lasers.

As will be described in more detail below, the gas inlet of the reactorassembly can be in fluid connection with at least one gas supplyselected from the group consisting of air, oxygen, hydrogen, helium,nitrogen, neon, argon, krypton, xenon, carbon monoxide, carbon dioxideand mixtures thereof; wherein the gas supply is free of metal salts andvaporized metals; and/or (iii) the gas supply is directed through a gasmanifold controlled by mass flow meters.

As will be described in more detail below, the nanoporous carbon powdercharged to the reactor assembly can comprise graphene having at least95% wt. carbon (metals basis), a mass mean diameter between 1 μm and 5mm, and an ultramicropore surface area between about 100 and 3000 m²/g.The nanoporous carbon powder is preferably characterized by acidconditioning, wherein the acid is selected from the group consisting ofHCl, HF, HBr, HI, sulfuric acid, phosphoric acid, carbonic acid, andnitric acid, and a residual water content of less than that achievedupon exposure to a relative humidity (RH) of less than 40% RH at roomtemperature.

As will be described in more detail below, the reactor assemblycomprises a plurality of devices that can impart electromagnetic fields,including x-ray sources, coils, lasers and lamps or lights, includingpencil lamps, short wave and long wave lamps. The wavelengths generatedby each device (e.g., lamps or lasers) can be independently selected.

As will be described in more detail below, the RA coils can be made fromthe same or different electrically conducting materials For example, afirst RA coil comprises a copper wire winding, a second RA coilcomprises a braiding of copper wire and silver wire, and a third RA coilis a platinum wire winding and each RA coil is configured to create amagnetic field and wherein each power supply independently provides ACand/or DC current.

As will be described in more detail below, the reactor assembly ispreferably characterized by (i) a first pair of RA lamps configured in afirst plane defined by a center axis and a first radius of the reactorchamber, (ii) a second pair of RA lamps configured in a second planedefined by the center axis and a second radius of the reactor chamberand (iii) a third pair of RA lamps configured in a third plane definedby the center axis and a third radius of the reactor chamber.Preferably, each RA lamp is a pencil lamp characterized by a tipsubstantially equidistant from the central axis and each pair of RAlamps comprises a vertical RA lamp and a horizontal RA lamp. Preferablyeach pair of lamps is equidistantly spaced around the circumference ofthe reactor chamber.

As will be described in more detail below, the reactor assembly furthercomprises an electromagnetic embedding enclosure (E/MEE or EMEE), asdefined more specifically below. The E/MEE is typically located along agas line upstream of the reactor assembly gas inlet. Typically, anelectromagnetic embedding enclosure located upstream of the gas inletcomprises:

-   -   (a) a gas inlet;    -   (b) at least one E/MEE pencil lamp positioned below the internal        gas line, at least one E/MEE pencil lamp positioned above the        internal gas line and at least one E/MEE pencil lamp positioned        to the side of the internal gas line;    -   wherein each E/MEE pencil lamp is independently rotatably        mounted, located along the length of the internal gas line, and    -   the lamps and/or coil(s) are powered by a power supply,        preferably the power supply of the reactor assembly;    -   the gas flow, lamps and/or coil(s) are preferably independently        controlled by one or more central processing units, preferably        the central processing unit (CPU) of the reactor assembly.        Typically, a CPU independently controls powering each E/MEE        pencil lamp and a rotation position of each E/MEE pencil lamp.

As will be described in more detail below, the E/MEE housing can betypically closed and opaque, the internal gas line can be transparentand external gas line in fluid connection with the housing outlet andgas inlet can be opaque. Typically, the internal gas line is between 50cm and 5 meters or more and has a diameter between 2 mm and 25 cm ormore.

As will be described in more detail below, the apparatus can have atleast 5 E/MEE pencil lamps located along the internal gas line. EachE/MEE pencil lamp can be independently placed such that its longitudinalaxis is (i) parallel to the internal gas line, (ii) disposed radially ina vertical plane to the internal gas line, or (iii) perpendicular to theplane created along the longitudinal axis of the internal gas line oralong the vertical axis of the internal gas line. Each E/MEE pencil lampcan be independently affixed to one or more pivots that permit rotationbetween about 0 and 360 degrees with respect to the x, y, and/or z axiswherein (i) the x-axis is defined as the axis parallel to the gas lineand its vertical plane, (ii) the y-axis defining the axis perpendicularto the gas line and parallel to its horizontal plane, and (iii) thez-axis is defined as the axis perpendicular to the gas line and parallelto its vertical plane.

As will be described in more detail below, at least one E/MEE pencillamp can be a neon lamp, at least one E/MEE pencil lamp can be a kryptonlamp, and at least one E/MEE pencil lamp can be an argon lamp. It can bedesirable to match, or pair, one or more E/MEE pencil lamps with one ormore (e.g., a pair) of RA lamps. Accordingly, at least one pair of RApencil lamps can be selected from the group consisting of a neon lamp, akrypton lamp and an argon lamp.

As will be described in more detail below, the invention includes aprocess of producing a nanoporous carbon composition comprising thesteps of:

-   -   (a) initiating a gas flow in a reactor assembly as described        herein;    -   (b) independently powering each RA coil to a first        electromagnetic energy level;    -   (c) powering the one or more RA frequency generators and        applying a frequency to each RA coil;    -   (d) independently powering each RA lamp;    -   (e) independently powering each laser;    -   (f) powering the x-ray source; and    -   (g) subjecting the nanoporous carbon powder to harmonic        electromagnetic resonance in ultramicropores of the nanoporous        carbon powder to instantiate an elemental metal nanostructure in        a nanopore.

The invention also includes a process of producing a nanoporous carboncomposition comprising the steps of:

-   -   (a) initiating a gas flow in a reactor assembly further        comprising an E/MEE, as described herein;    -   (b) independently powering each RA coil to a first        electromagnetic energy level;    -   (c) powering the one or more RA frequency generators and        applying a frequency to each RA coil;    -   (d) independently powering each RA lamp;    -   (e) independently powering each laser;    -   (f) powering the x-ray source; and    -   (g) subjecting the nanoporous carbon powder to harmonic        electromagnetic resonance in ultramicropores of the nanoporous        carbon powder to instantiate an elemental metal nanostructure in        a nanopore.

The invention also includes a process of instantiating an elementalmetal within an ultramicropore of a nanoporous carbon powder comprisingthe steps of:

-   -   (a) initiating a gas flow in a reactor assembly further        comprising an E/MEE, as described herein;    -   (b) independently powering each RA coil to a first        electromagnetic energy level;    -   (c) powering the one or more RA frequency generators and        applying a frequency to each RA coil;    -   (d) independently powering each RA lamp;    -   (e) independently powering each laser;    -   (f) powering the x-ray source; and    -   (g) subjecting the nanoporous carbon powder to harmonic        electromagnetic resonance in ultramicropores of the nanoporous        carbon powder to instantiate an elemental metal nanostructure in        a nanopore.

The invention also includes a process of quantum printing an elementalmetal within a nanoporous carbon powder comprising the steps of:

-   -   (a) initiating a gas flow in a reactor assembly further        comprising an E/MEE, as described herein;    -   (b) independently powering each RA coil to a first        electromagnetic energy level;    -   (c) powering the one or more RA frequency generators and        applying a frequency to each RA coil;    -   (d) independently powering each RA lamp;    -   (e) independently powering each laser;    -   (f) powering the x-ray source; and    -   (g) subjecting the nanoporous carbon powder to harmonic        electromagnetic resonance in ultramicropores of the nanoporous        carbon powder to instantiate an elemental metal nanostructure in        a nanopore.

As will be described in more detail below, the invention also includesnanoporous carbon powder compositions and metal compositions produced inaccordance with the claimed methods and processes.

BRIEF DESCRIPTION OF THE DRAWINGS

The patent or application file contains at least one drawing executed incolor. Copies of this patent or patent application publication withcolor drawing(s) will be provided by the Office upon request and paymentof the necessary fee.

The foregoing and other objects, features and advantages of theinvention will be apparent from the following more particulardescription of preferred embodiments of the invention, as illustrated inthe accompanying drawings in which like reference characters refer tothe same parts throughout the different views. The drawings are notnecessarily to scale, emphasis instead being placed upon illustratingthe principles of the invention.

FIG. 1 is a perspective view of an E/MEE of the invention.

FIGS. 2A and 2C show reactor assembly components. FIG. 2B is an expandedview of the reactor assembly components of FIG. 2A.

FIG. 3A, FIG. 3B, FIG. 3C, FIG. 3D and FIG. 3E provides five views ofcoils which can be used in a reactor assembly.

FIG. 4A is a perspective view of an E/MEE of the invention used incarbon pretreatment. FIG. 4B shows reactor assembly components.

FIG. 5A illustrates one conformation for a standard coil. FIG. 5Billustrates one conformation for a reverse field coil.

FIGS. 6A and 6B are illustrations of two examples of two compositereactor assemblies. FIG. 6A illustrates a Composite Reactor with acopper body, carbon graphite cup and a carbon graphite cap. FIG. 6Billustrates a Composite Reactor with a carbon graphite body and cap andmetal foil boundary.

FIG. 7 is a graph illustrating process performance as a function ofultra-micro pore surface area. Performance is defined as a postcondition having greater than 5 sigma change in instantiation/nucleationproduction compared to the pre-condition.

FIGS. 8A, 8B, 8C and 8D are SEMs of a metal macrostructure comprisingagglomerated metal nanostructures and illustrate nanowires, threads andcoils.

FIGS. 9A and 9B illustrate macrostructure comprising agglomeratednanoparticles with a nugget morphology. FIGS. 9A and 9B arepredominantly copper with a significant amount of surface platinum(Illustration 2). FIG. 9C is an SEM of a platinum-containingmacrostructure and clearly depicts instantiation from a carbon poreproduced in Illustration 31. FIG. 9D is a copper-containing wire.Ytterbium was also identified in this run. FIG. 9E clearly illustratesthe agglomerated nanostructures in a macrostructure.

FIG. 10A illustrates agglomeration. FIG. 10B illustrates the diversityof elemental metals that can be detected in a metal macrostructure. Thissample was isolated from Illustration 2. FIG. 10C is an image of themacrostructure product isolated from Illustration 2. The entire image isapproximately 40 nm by 40 nm. The yellow, or lighter areas, at the topof the figure are predominantly carbon (internal to the macrostructure)while the blue or darker areas at the lower left corner arepredominantly copper. The image suggests assembly and condensation ofcopper on and within the carbon. FIGS. 10D and 10E are Titan TEM imagesof the carbon copper interface. Note the scales. Yellow or the lightestcolor depicts carbon. Rows of red (or medium gray) copper atoms can beidentified in the center of the image in FIG. 10D and a lighter carbon“hole” can be identified in the lower right quadrant. Copper rich carbonregions can be seen in red (medium grey), for example in the lower leftquadrant of FIG. 10D. The bottom left corner is blue (or dark grey) anddetects high purity copper in a macrostructure of the invention. In FIG.10E, copper is identified in a bottom banner while carbon is in the topbanner. At the interface, the assembly and condensation of copper withinthe carbon can be seen. FIG. 10F is a Focused Ion Beam (FIB) slice of acopper nugget isolated from Illustration 2. Note the internal voids.FIG. 10G illustrates patterned growth, e.g., rows, contours, ringsand/or circles, the latter resembling rings on a cut tree stump, on amacroscale. Note the patterning of the morphology deposited in thecenter, resembling a rose.

FIG. 11 illustrates the nucleation of elemental nanostructures. Thephotograph clearly shows graphite like and graphene sheets and rodsprotruding from within a graphene pore. The rods are silicon calcium inthis photo. To the right of the photograph, titanium nanospheres inlight grey can be identified.

FIG. 12 shows a silicon dioxide particle identified in a nanoporouscarbon composition. A rectangle was removed from the particle surface,exposing aggregated nanostructure.

FIG. 13A, FIG. 13B and FIG. 13C show images of internal voids of a metaldeposit or metal macrostructure of the invention. FIG. 13D is aphotograph of a macrostructure obtained from Illustration 12. Thephotograph was obtained using an optical microscope.

FIG. 14A, FIG. 14B, and FIG. 14C shows SEM images of clathrates. FIG.14D shows a SEM image of a metal organic framework.

FIG. 15A, FIG. 15B, FIG. 15C, FIG. 15D, FIG. 15E, FIG. 15F, FIG. 15G,FIG. 15H and FIG. 15I illustrate various reactor assembly viewsaccording to the invention.

FIG. 16A, FIG. 16B, FIG. 16C, FIG. 16D and FIG. 16E are periodic tablesillustrating elements detected in the carbon matrices produced by theprocesses of the invention and exemplified herein.

FIG. 17A, FIG. 17B and FIG. 17C are illustrations of reactor variations.

FIG. 18A and FIG. 18B are an artist's rendition of nanoporous carboncompositions. Interconnecting pores are shown as columns connectinglayers while the ultramicropores are shown extending from the pores.Optional surface chemistry is illustrated as CO₂, H₂O and ChemicalMoieties. Electromagnetic (EM) jets are illustrated showing harmonicresonances established within the pores.

DETAILED DESCRIPTION

The invention relates to methods of instantiating materials, such asmetals, in nanoporous carbon powders. The invention includes methodscomprising the steps of contacting a bed comprising a nanoporous carbonpowder with a gas, and optionally an electromagnetically activated gas,while applying electromagnetic radiation to the nanoporous carbon powderfor a time sufficient to cause instantiation, including nucleation andagglomeration, of elemental metal nanoparticles within and/or fromcarbon nanopores. The process results in a composition comprising ananoporous carbon powder characterized by (i) elemental metalnanoparticles deposited within carbon nanopores and/or (ii)agglomerated, or aggregated, elemental metal nanoparticles, creatingmacrostructures such as elemental metal nuggets, nanowires and othermacrostructures that can be easily separated from the nanoporous carbonpowder. The processes of the invention have broad applicability inproducing elemental metal macrostructures. The invention further relatesto the nanoporous carbon compositions, elemental metal nanoparticles andelemental metal macrostructures produced by the methods of theinvention.

The use of the terms agglomeration and aggregation is not intended toinfer a specific order of assembly of the macrostructures. That is, itis not assumed that discrete nanoparticles are formed and then relocateand assemble to form an aggregate, as may be considered common in powderhandling with electrostatically assembled products. Rather, withoutbeing bound by theory, it is believed that the agglomeration oraggregation occurs as nanoparticles are formed in ultramicropores.

The invention contemplates compositions comprising a nanoporous carbonpowder comprising (a) nanopores having disposed therein elemental metalnanostructures and (b) an elemental metal macrostructure wherein theelemental metal macrostructure further comprises internal carbon.

Nanoporous Carbon Powders

Nanoporous carbon powders or nanostructued porous carbons can be used inthe processes and methods of the invention. Nanoporous carbon powders ornanostructued porous carbons are also referred to herein as “startingmaterial” or “charge material”. The carbon powder preferably provides asurface and porosity (e.g., ultra-microporosity) that enhances metaldeposition, including deposit, instantiation and growth. Preferredcarbon powders include activated carbon, engineered carbon, graphite,and graphene. For example, carbon materials that can be used hereininclude graphene foams, fibers, nanorods, nanotubes, fullerenes, flakes,carbon black, acetylene black, mesophase carbon particles, microbeadsand, grains. The term “powder” is intended to define discrete fine,particles or grains. The powder can be dry and flowable or it can behumidified and caked, such as a cake that can be broken apart withagitation. Although powders are preferred, the invention contemplatessubstituting larger carbon materials, such as bricks and rods includinglarger porous carbon blocks and materials, for powders in the processesof the invention.

The examples used herein typically describe highly purified forms ofcarbon, such as >99.995% wt. pure carbon (metals basis). Highly purifiedforms of carbon are exemplified for proof of principal, quality controland to ensure that the results described herein are not the result ofcross-contamination or diffusion within the carbon source. However, itis contemplated that carbon materials of less purity can also be used.Thus, the carbon powder can comprise at least about 95% wt. carbon, suchas at least about 96%, 97%, 98% or 99% wt. carbon. In a preferredembodiment, the carbon powder can be at least 99.9%, 99.99% or 99.999%wt. carbon. In each instance, purity can be determined on either an ashbasis or on a metal basis. In another preferred embodiment, the carbonpowder is a blend of different carbon types and forms. In oneembodiment, the carbon bed is comprised of a blend of differentnano-engineered porous carbon forms. Carbon powders can comprisedopants. Dopants can be measured in the carbon powder starting materialsby the same techniques as can measure the elemental metal nanostructuresas described below. Applicants believe that metal, semi-metal andnon-metal dopants can impact the formation of elemental metalnanostructures.

The carbon powder preferably comprises microparticles. The volume mediangeometric particle size of preferred carbon powders can be between lessthan about 1 μm and 5 mm or more. Preferred carbon powders can bebetween about 1 μm and 500 μm, such as between about 5 μm and 200 μm.Preferred carbon powders used in the exemplification had mediandiameters between about 7 μm and 13 μm and about 30 μm and 150 μm.

The dispersity of the carbon particle size can improve the quality ofthe products. It is convenient to use a carbon material that ishomogeneous in size or monodisperse. Thus, a preferred carbon ischaracterized by a polydispersity index of between about 0.5 and 1.5,such as between about 0.6 and 1.4, about 0.7 and 1.3, about 0.8 and 1.2,or between about 0.9 and 1.1. The polydispersity index (or PDI) is theratio of the mass mean diameter and number average diameter of aparticle population. Carbon materials characterized by a bimodalparticle size can offer improved gas flow in the reactor.

The carbon powder is preferably porous. The pores, or cavities, residingwithin the carbon particles can be macropores, micropores, nanoporesand/or ultra-micropores. A pore can include defects in electrondistribution, compared to graphene, often caused by changes inmorphology due to holes, fissures or crevices, corners, edges, swelling,or changes in surface chemistry, such as the addition of chemicalmoieties or surface groups, etc. For example, variation in the spacesthat may arise between layers of carbon sheets, fullerenes or nanotubesare contemplated. It is believed that deposit instantiationpreferentially occurs at or within a pore or defect-containing pore andthe nature of the surface characteristics can impact the deposit. Forexample, Micromeritics enhanced pore distribution analysis (e.g., ISO15901-3) can be used to characterize the carbon. It is preferred thatthe carbon powder is nanoporous. A “nanoporous carbon powder” is definedherein as a carbon powder characterized by nanopores having a poredimension (e.g, width or diameter) of less than 100 nm. For example,IUPAC subdivides nanoporous materials as microporous (having porediameters between 0.2 and 2 nm), mesoporous materials (having porediameters between 2 and 50 nm) and microporous materials (having porediameters between 50 nm and 1000 nm). Ultramicropores are defined hereinas having pore diameters of less than about 1 nm.

Uniformity in pore size and/or geometry is also desirable. For example,ultramicropores in preferred carbon materials (e.g., powders) accountfor at least about 10% of the total porosity, such as at least about20%, at least about 30%, at least about 40%, at least about 50%, atleast about 60%, at least about 70%, at least about 80%, or at leastabout 90%. Preferred carbon materials (e.g., powders) are characterizedwith a significant number, prevalence or concentration ofultra-micropores having the same diameter, thereby providing predictableelectromagnetic harmonic resonances and/or standing wave forms withinthe pores, cavities, and gaps. The word “diameter” in this context isnot intended to require a spherical geometry of a pore but is intendedto embrace a dimension(s) or other characteristic distances betweensurfaces. Accordingly, preferred carbon materials (e.g., powders) arecharacterized by a porosity (e.g., nanopores or ultramicropores) of thesame diameter account for at least about 10% of the total porosity, suchas at least about 20%, at least about 30%, at least about 40%, at leastabout 50%, at least about 60%, at least about 70%, at least about 80%,or at least about 90%.

Measuring adsorption isotherm of a material can be useful tocharacterize the surface area, porosity, e.g., external porosity, of thecarbon material. Carbon powders having a surface area between about 1m²/g and 3000 m²/g are particularly preferred. Carbon powders having anultramicropore surface area of at least about 50 m²/g, preferably atleast about 300 m²/g, at least about 400 m²/g, at least about 500 m²/gor higher are particularly preferred. Activated or engineered carbons,and other quality carbon sources, can be obtained with a surface areaspecification. Surface area can be independently measured by BET surfaceadsorption technique.

Surface area correlation with metal deposition was explored in a numberof experiments. Classical pore surface area measurements, usingMicromeritics BET surface area analytical technique with nitrogen gas at77K (−196.15 C) did not reveal a substantial correlation in thedeposition of elements at ≥5σ confidence level, or probability ofcoincidence. However, a correlation with ultramicropores (pores having adimension or diameter of less than 1 nm) was observed. Carbon dioxideadsorption at 273K (0 C) was used to assess ultra-microporosity. Asshown in FIG. 7, performance, as measured by successful nucleation orinstantiation, correlated with ultra-microporosity. Without being boundby theory, instantiation is believed to be correlated to resonatingcavity features of the ultra-micropore and ultramicropore network suchas the distance between surfaces or walls. Features of theultramicropore, can be predicted from ultramicropore diameter asmeasured by BET, augmented by density function theory (DFT) models, forexample. With the aid of machine learning, more precise relationshipsbetween ultramicropore size, distribution, turbostratic features, wallseparation and diameter and elemental metal nucleation can beestablished.

Carbon materials and powders can be obtained from numerous commercialproviders. MSP-20X and MSC-30 are high surface area alkali activatedcarbon materials with nominal surface areas of 2,000-2,500 m²/gand >3,000 m²/g and median diameters of 7-13 μm and 60-150 μmrespectively (Kansai Coke & Chemicals Co). Norit GSX is a steam-washedactivated carbon obtained from Alfa Aesar. The purified carbon formsused in the experimental section all exceed ≥99.998_(wt)% C (metalsbasis).

Modifying the surface chemistry of the carbon can also be desirable. Forexample, improved performance was observed when conditioning the carbonwith an acid or base. Contacting the carbon with a dilute acid solutionselected from the group consisting of HCl, HF, HBr, HI, sulfuric acid,phosphoric acid, carbonic acid, and nitric acid followed by washing withwater (such as deionized water) can be beneficial. The acid ispreferably in an amount less than about 30%, less than about 25%, lessthan about 20% less than about 15%, less than about 10%, or less thanabout 5%, preferably less than or equal to 1% vol. The preferred acidfor an acid wash is an acid having a pKa of less than about 3, such asless than about 2. After washing, it can be beneficial to subject thecarbon to a blanket of an inert gas, such as helium, hydrogen ormixtures thereof. Alternative gases include carbon monoxide, carbondioxide, nitrogen, argon, neon, krypton, helium, ammonia and hydrogen.The carbon can also be exposed to a base, such as KOH before or after anacid treatment.

Controlling residual water content in the carbon which may includemoisture can improve performance. For example, the carbon material canbe placed in an oven at a temperature of at least about 100° C.,preferably at least about 125° C., such as between 125° C. and 300° C.for at least 30 minutes such as about an hour. The oven can be atambient or negative pressure, such as under a vacuum. Alternatively, thecarbon material can be placed in an oven with high vacuum at atemperature of at least about 250° C., preferably at least about 350°C., for at least one hour, such as at least 2, 3, 4, 5, or 6 hours.Alternatively, the carbon material can be placed in an oven with highvacuum at a temperature of at least about 700° C., preferably at leastabout 850° C., for at least one hour, such as at least 2, 3, 4, 5, or 6hours. Alternatively, the water or moisture can be removed by vacuum orlyophilization without the application of substantial heat. Preferably,the water, or moisture, level of the carbon is less than about 35%, 30%,25%, 20%, 15%, 10%, 5%, such as less than about 2%, by weight carbon. Inother embodiments, the carbon can be exposed to a specific relativehumidity (RH) such as 5%, 12% RH or 40% RH or 70% RH or 80% RH or 90%RH, for example, at 22° C.

Pre-treatment of the carbon material can be selected from one or more,including all, the steps of purification, humidification, activation,acidification, washing, hydrogenation, drying, chemistry modification(organic and inorganic), and blending. For example, the carbon materialcan be reduced, protonated or oxidized. The order of the steps can be asdescribed, or two or more steps can be conducted in a different order.

For example, MSP-20X was exposed to an alkali (C:KOH at a molar ratio of1:0.8), activated at 700° C. for 2 hours, washed with acid and thenhydrogenated to form MSP-20X Lots 1000 when washed with HCl and 105 whenwashed with HNO3. MSP-20X was washed with acid and then hydrogenated toform MSP-20X Lots 1012 when washed with HCl and 1013 when washed withHNO3. Activated carbon powder developed for the storage of hydrogen wasHCl acid washed, then subjected to HNO3 washing and hydrogenation toform APKI lots 1001 and 1002, as substantially described in Yuan, J.Phys. Chem. B20081124614345-14357]. Poly(ether ether ketone) (PEEK,Victrex 450P) and poly(ether imide) (PEI, Ultem® 1000) was supplied bythermally oxidized in static air at 320° C. for 15 h, and carbonized atthe temperature range of 550-1100° C. in nitrogen atmosphere, at thecarbon yield of 50-60 wt %. These carbons were then activated by thefollowing procedures: (1) grind the carbonized polymer with KOH atKOH/carbon ˜ 1/1-1/6 (w/w), in the presence of alcohol, to form a finepaste; (2) heat the paste to 600-850° C. in nitrogen atmosphere for 2 h;(3) wash and rinse with DI water and dry in vacuum oven. PEEK/PEI (50/50wt) blend was kindly supplied by PoroGen, Inc. Likewise, the acidwashing sequence of Lots 1001 and 1002 was reversed to form APKI lots1003 and 1004. Universal grade, natural graphite, ˜200 mesh waspurchased from Alfa Aesar, product number 40799. Graphite lots R and Zwere HCl washed and hydrogenated to form R lot 1006 and Z lot 1008,respectively. Alfa Aesar graphite R and Z were nitric acid washed andhydrogenated to form R lot 1007 and Z lot 1009, respectively. MSC-30(Kansai Coke and Chemicals) was acid washed and then hydrogenated toform MSC30 lots 1010 when washed with HCl and 1011 when washed withHNO3. MSC-30 was exposed to an alkali (C:KOH at a molar ratio of 1:0.8),activated at 700 C for 2 hours, HCl or nitric acid washed and thenhydrogenated to form MSC-30 lots 1014 (HCl washed) and 1015 (HNO3washed), respectively. MSP-20X, MSC-30, Norit GSX and Alfa Aesar R weresubjected to purification by MWI, Inc. for MSP-20X Lots 2000 and 2004,MSC-30 Lots 2001, 2006 and 2008, Norit GSX Lots 2005 and 2007, and AlfaAesar R Lot 2009 respectively. MSP-20X Lot 2000 and MSC-30 2001 were HClwashed and hydrogenated to form MSP-20X Lot 2002 and MSC-30 Lot 2003,respectively. Alfa Aesar R was washed with 1%, 5%, 10%, 15%, 20%, 25%,and 30% HCl (vol.) and then hydrogenated to for R Lot Graphite n % volHCl, respectively. Purified MSP-20X (Lot 2006) was similarly washed byHCl, nitric acid, HF or H₂SO₄ to form MSP-20X 1% HCl, MSP-20X 1% HNO3,MSP-20X 0.4% HF, MSP-20X 0.55% H₂SO₄ (Lot 1044), respectively. PurifiedNorit GSX (Lot 2007) was similarly washed by nitric acid, HF or H₂SO₄ toform Norit GSX 1% HNO3 (Lot 1045), Norit-GSX 0.4% HF, Norit-GSX 0.55%H₂SO₄, respectively. Purified MSC30 (Lot 2008) was similarly washed byHCl and H₂SO₄ to form MSC30 1% HCl, and MSC30 5% H₂SO₄. Purified MSP20X(Lot 2006), Norit GSX (Lot 2007) and MSC30 (Lot 2008) were hydrogenated.Purified MSP-20X, Norit GSX and MSC30 were washed with 1% HCl usingmethanol as a wetting agent. APKI-S-108 Lots 1021-1024 were recycled.The Ref-X Blend is a 40% Alfa Aesar R: 60% MSP-20X (lot 2006) 850° C.desorb then CO₂ exposure at 138 kPa (20 psi) for 5 days.

The carbon can be recycled or reused after the metal deposit has beenrecovered from the process. In recycling the carbon, the carbon canoptionally be subjected to an acid wash and/or water removal one or moretimes. In this embodiment, the carbon can be reused one or more times,such as 2, 3, 4, 5, 10, 15, 20, or about 25 or more times. The carboncan also be replenished in whole or in part. It has been discovered thatrecycling or reusing the carbon can enhance metal nanostructure yieldsand adjust nucleation characteristics enabling change in elementselectivity and resultant distributions. Thus, an aspect of theinvention is to practice the method with recycled nanoporous carbonpowder, e.g., a nanoporous carbon powder that has been previouslysubjected to a method of the invention one or more times.

Nanoporous Carbon Compositions and Metal Deposits

The nanoporous carbon compositions produced by the processes describedherein possess several surprising and unique qualities. The nanoporosityof the carbon powder is generally retained during processing and can beconfirmed, for example, visually with a scanning electron microscope orby BET. Visual inspection of the powder can identify the presence ofelemental nanostructures residing within and surrounding the nanopores.The nanostructures are typically elemental metals. Visual inspection ofthe powder can also identify the presence of elemental macrostructuresresiding within and surrounding the nanopores. The macrostructures aretypically elemental metals and often contain interstitial and/orinternal carbon.

The metal nanostructures and/or metal macrostructures (collectively,“metal deposits”) produced by the process can be isolated or harvestedfrom nanoporous carbon compositions. The metal deposits of the inventionalso possess several surprising and unique qualities.

Typically, the porosity of the nanoporous carbon compositions will be atleast about 70% of the porosity attributed to ultramicropores of thenanoporous carbon powder starting, or charge, material and having atotal void volume that is about 40% or more of the bulk material volume.The pores, or cavities, residing within the carbon particles can bemacropores, micropores, nanopores and/or ultra-micropores. A pore caninclude defects in electron distribution, compared to graphene, oftencaused by changes in morphology due to holes, fissures or crevices,edges, corners, swelling, dative bonds, or other changes in surfacechemistry, such as the addition of chemical moieties or surface groups,etc. For example, the spaces that may arise between layers of carbonsheets, fullerenes, nanotubes, or intercalated carbon are contemplated.It is believed that deposit and instantiation preferentially occurs ator within a pore and the nature of the surface characteristics canimpact the deposit. For example, Micromeritics enhanced poredistribution analysis (e.g., ISO 15901-3) can be used to characterizethe carbon. It is preferred that the carbon powder is nanoporous.

The products can also be characterized by uniformity in pore size and/orgeometry. For example, ultramicropores can account for at least about10% of the total porosity, such as at least about 20%, at least about30%, at least about 40%, at least about 50%, at least about 60%, atleast about 70%, at least about 80%, or at least about 90%. Carbonmaterials (e.g., particles or powders) can be characterized with asignificant number, prevalence or concentration of ultra-microporeshaving the same dimension (e.g., width or diameter) or the samedistribution of pore dimensions or dimensions characterizing the porenetwork, thereby providing predictable electromagnetic harmonicresonances within the pores. Accordingly, carbon materials (e.g.,powders) can be characterized by a porosity (e.g., nanopores orultramicropores)) of the same diameter or diameter distribution accountfor at least about 10% of the total porosity, such as at least about20%, at least about 30%, at least about 40%, at least about 50%, atleast about 60%, at least about 70%, at least about 80%, or at leastabout 90%.

Measuring surface area of a material can be useful to characterize theporosity, e.g., external porosity, of the carbon material. The carbonpowder preferably is characterized by a high surface area. For example,the nanoporous carbon powder can have a general surface area of at leastabout 1 m²/g or at least about 200 m²/g, at least about 500 m²/g or atleast about 1000 m²/g. The ultra-micropore surface area can be at leastabout 50 m²/g, such between 100 m²/g and 3,000 m²/g. The ultramicroporesurface area of at least about 50 m²/g, preferably at least about 300m²/g, at least about 400 m²/g, at least about 500 m²/g or higher areparticularly preferred. Activated carbons, and other quality carbonsources, can be obtained with a surface area specification. Surface areacan be independently measured by BET surface adsorption technique.

Carbon materials (e.g., powders and particles) include activated carbon,engineered carbon, natural and manufactured graphite, and graphene. Forexample, carbon materials that can be used herein includemicroparticles, graphene foams, fibers, nanorods, nanotubes, fullerenes,flakes, carbon black, acetylene black, mesophase carbon particles,microbeads and, grains. Typically, a powder can be sufficiently dry tobe flowable without substantial aggregation or clumping or it can behumidified and caked, such as a cake that can be broken apart withagitation. Although powders are preferred, the invention contemplatessubstituting larger carbon materials, such as bricks and rods, forpowders in the processes of the invention.

Typically, the sp²-sp³ character of the carbon composition (e.g., theinternal carbon) changed as carbon rich to metal rich structures wastraversed, as determined by TEM-EELs (transition electronmicroscopy—electron energy loss spectroscopy).

The nanoporous carbon compositions are typically characterized by thepresence of “detected metals,” or a “reduced purity,” as compared to thenanoporous carbon powder starting material, as determined by X-rayfluorescence spectrometry (XRF) using standardized detection methods.ED-XRF and WD-XRF can be used. In addition, Energy DispersiveSpectroscopy (EDS or EDX or HR-Glow Discharge Mass Spectrometry (GD-MS)as well as Neutron Activation Analysis (NAA), Parr Bomb Acid Digestionwith ICP-MS, PIXE and GD-OES can be used in addition, in the alternativeor in any combination. For example, in the experimentation describedbelow, carbon materials with a purity of at least 99.9% by weight wasused as an initial starting material and most typically at least 99.99%by weight on a metals basis. Such carbon materials can comprise small(e.g., <1% by weight) metals, or dopants. Such pre-existing metals,including dopants, are not included within the “detected metals”definition. Products of the invention were characterized by depositedelemental metal nanostructures and nano-deposits that were detected byXRF, EDS/EBSD and other methods. The resulting carbon powder productscharacterized by such metal deposits can be characterized as having a“reduced purity.” The term, “detected metals,” is defined herein toexclude any element or material introduced by the carbon startingmaterial, gas supply, gas line, or reactor assembly, including thereactor frits, cup and/or cap (collectively “reactor components”). Byway of an example, where the reactor is selected from a copper cup whichcontains the carbon material, and the process results in a massreduction of 1 μg of copper from the cup, then a “detected metal”excludes 1 μg copper. In addition, the elemental composition(s) of thereactor components and reactor feed gas can be compared to the detectedmetals. Where the reactor components differ in elemental composition,the detection of one or more metals not present in any of the reactorcomponents supports the conclusion that the detected metal is notderived from the reactor components. For example, where the detectedmetal contains 5 ppm wt Mo or 4 ppm wt W in addition to copper within anelemental metal macrostructure, and the reactor cup is 99.999% copperwith no detectable Mo or W, the copper identified within the detectedmetal can also be attributed to the total detected metals. Typically, atleast about 1% of the total non-carbon elements contained within thecarbon composition are detected metals or components, on a mass basis.Preferably, detected metals are at least about 2%, 3%, 4%, 5%, 6%, 7%,8%, 9%, 10%, 20%, 30%, 40%, 50%, 60% or 70% or more of the totalnon-carbon elements contained within the carbon composition on a massbasis.

In a preferred embodiment, the nanoporous carbon composition comprisesat least 0.1 ppm detected metal, preferably between about 0.1 ppm-100ppm, such as between about 50 ppm-5000 ppm, or between about 0.1% wt-20%wt, such as at least about >0.1% wt detected metals. Preferably thedetected metals are at least 1 ppm of the nanoporous carbon composition.The detected metals can be, or include, the elemental metalnanostructures (or, simply metal nanostructures). The detected metalsexclude metal ions or salts.

Carbon compositions subjected to the methods of the invention result inan altered carbon isotopic ratio. Thus, the invention includes methodsof altering the carbon isotopic ratio comprising eh steps describedbelow and compositions wherein the carbon isotopic ration has shifted.

The nanoporous carbon composition preferably comprises elemental metalnanostructures. The metal nanostructures preferably comprise one or moremetals selected from the group consisting of transition metals (GroupSc, Y, Lu; Group IVB: Ti, Zr, Hf; Group VB: V, Nb, Ta; Group VIII Cr,Mo, W; Group VIIB: Mn, Re Group VIIIB: Fe, Ru, Os, Co, Rh, Ir, Ni, Pd,Pt; Group IB: Cu, Ag; Group IIB: Zn, Cd, Hg), alkaline earth metals(Group Ia: Li, Na, K, Rb, Cs), alkali metals (Group IIA: Be, Mg, Ca, Sr,Ba), lanthanides (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm andYb), and light metals (B, Al, Si, S, P, Ga, Ge, As, Se, Sb, Te, In, Tl,Sn, Pb, Bi). Platinum group metals and rare earth elements arepreferred. Precious metals and noble metals can also be made. Othernanostructures comprising Li, B, Si, P, Ge, As, Sb, and Te can also beproduced. Typically, the elemental metal nanostructures exclude metalions.

The nanoporous carbon composition can also comprise non-metalnanostructures and/or macrostructures. For example, the processes of theinvention can instantiate or quantum print gases, such as hydrogen,oxygen, helium, neon, argon, krypton and xenon. Additionally oralternatively, the invention can instantiate or quantum print materialscontaining carbon, oxygen, nitrogen, sulfur, phosphorous, selenium,hydrogen, and/or halides (e.g., F, Cl, Br and I). Nanoporous carboncompositions further comprising metal oxides, nitrides, hydrides, andsulfides such as copper oxide, molybdenum sulfide, aluminum nitride havebeen identified. Therefore, small inorganic molecules or compounds(e.g., molecules comprising several metal atoms, e.g., 2, 3, 4, 5, 6, 7,8, 9 or 10 atoms) can be instantiated or printed using the processes ofthe invention. Examples of such small molecules include carbides,oxides, nitrides, sulfides, phosphides, halides, carbonyls, hydroxides,hydrates including water, clathrates, clathrate hydrates, and metalorganic frameworks (FIG. 14A, FIG. 14B, FIG. 14C, FIG. 14D). FIG. 10A isan SEM close-up of a macrostructure isolated from Illustration 2. FIG.10B provides an example of the detected elemental diversity of themacrostructure typical of products produced by the processes. Thus, theinvention relates to metal macrostructures characterized by 3, 4, 5, 6,7, 8, 9, 10 or more elemental metals. Preferred metal macrostructurescomprise a preponderance of an elemental metal. A metal is“preponderant” within a macrostructure where the elemental weightcontent is substantially greater than one, two or more, or all of theother detected metals. For example, at least about 50%, 60%, 70%, 80%,90% or more of the macrostructure comprises a preponderant elementalmetal. Macrostructures with a preponderance of copper, nickel, iron, andmolybdenum, have been isolated. Preferred macrostructures comprise apreponderance of a single element such as >95% copper, >95% Ni, >90%Mo, >90% Pt, and the like. Preferred macrostructures can also comprise apreponderance of 2 or more additional elemental metals. As also can beseen from FIG. 10B, the main, or preponderant, metal is copper.Preferred macrostructures comprise a preponderance of nickel, molybdenumand 3 or more additional elemental metals. Preferred macrostructurescomprise a preponderance of iron and molybdenum and 3 or more additionalelemental metals. Preferred macrostructures comprise a preponderance ofcopper and tungsten and 3 or more additional elemental metals. Preferredmacrostructures comprise preponderance of nickel, tungsten and 3 or moreadditional elemental metals. Preferred macrostructures comprise (i)platinum and 3 or more additional elemental metals, (ii) palladium and 3or more additional elemental metals, (iii) osmium and 3 or moreadditional elemental metals, or (iv) rhodium and 3 or more additionalelemental metals. It can be desirable, for the purposes ofcharacterizing the elemental composition of a macrostructure tonormalize the data against the preponderant metal. For example,XRF-spectra reported in this application are typically normalizedagainst the preponderant metal (e.g., copper, nickel, iron ormolybdenum). Accordingly, it is an aspect of the invention tocharacterize the elemental composition of a metal macrostructurenormalized against the most preponderant metal.

FIG. 10A is an SEM close-up of a macrostructure isolated fromIllustration 2. FIG. 10B provides the elemental diversity of themacrostructure. FIG. 10B provides an XRF spectra that is typical of theinvention.

FIG. 10C is a Titan TEM image showing sub-nanoscale structures, uniqueto the methods. Evidence of anisotropic copper growth originating from acarbon nano-reactor cavity (circle). Note the finger-like tendrils nearthe carbon/copper interface. These patterns are not found in typicaloxygen-free high-conductivity copper (OFHC). Thus, the inventionincludes a nanoporous carbon composition and metal deposits comprising acopper characterized by anisotropic tendril morphology at acarbon-copper interface.

FIGS. 10D and 10E are Titan TEM images of a carbon-copper interface ofthis copper macrostructure. Note the nanometer scales. Yellow, or thelightest color in black and white, depicts carbon. Rows of red copperatoms can be identified in the center of the image in FIG. 10D and alighter carbon “hole” can be identified in the lower right quadrant.Copper-rich carbon regions can be seen in red, or a grayer shade inblack and white, for example in the lower left quadrant of FIG. 10D. Thebottom left corner is blue, or black in black and white, and detectshigh purity copper. In FIG. 10E, copper is identified in a bottom bannerwhile carbon is in the top banner and a gradient of carbon and copperappears in the center. At the interface, the assembly and condensationof copper within the carbon can be seen. It is clear from these imagesthat the metal nanostructures comprise internal carbon. Therefore, theinvention includes elemental metal nanostructures and macrostructurescomprising internal carbon. It has been found that the carbon in themetal- or copper-rich regions (or otherwise at the carbon-metalinterface) are sp² carbon or graphite-like. The carbon appears to bemore amorphous in other regions, as detected by EELS and a K2 Summitcamera (Gatan). It is also clear from these images that ordered rows, oran array, of metal or copper atoms are deposited in the carbon, muchlike one would see from a printer. Thus, the invention further includesmethods of quantum printing elements within a nanoporous carbon powderand a nanoporous carbon powder characterized by discrete rows ofelemental metal atoms, such as copper. The copper island region that isshown in FIG. 10E was aligned with a CuO standard. Thus, the inventionfurther includes elemental metal (e.g., copper, platinum, platinum groupmetal or precious metal) nanostructures further comprising CuO andcarbon, particularly sp² carbon.

The processes of the invention result in a nanoporous carbon compositioncomprising an ordered metal nano-deposit array wherein the metalnano-deposits are characterized by a diameter of less than 1 nm,preferably between about 0.1 and 0.3 nm, and the space between the metaldeposit rows is less than about 1 nm, preferably between about 0.1 and0.3 nm. The nanoporous carbon composition comprising the ordered arrayis preferably characterized by a carbon rich area and/or a metal (e.g.,copper) rich adjacent to the array. For example, the array can belocated between a carbon-metal (e.g., copper) interface. The array canbe identified and characterized by tunneling electron microscopy (TEM).Typically, the TEM, and other microscopy devices, are used in accordancewith the manufacturer's instructions. The metal nano-deposit array ispresented (or located) on a carbon substrate wherein the carbonsubstrate preferably comprises sp² carbon. The term “nano-deposits” isintended to embrace nanostructures of less than about 1 nm and includesdiscrete atoms.

The processes of the invention result in a nanoporous carbon compositioncomprising a carbon-metal (e.g., copper) gradient wherein metal (e.g.,copper) nanostructures are deposited on a carbon substrate in gradientat a carbon-metal interface. The carbon substrate preferably comprisessp² carbon. The gradient is preferably about 100 nm, or about 50 nm orless in width, such as less than about 10 nm in width. The gradient isdefined by an increasing concentration of metal from a substantiallypure carbon region to a substantially carbon-free region. The metalregion can be characterized by an elemental composition consistent withthe metal nano-deposits described herein.

FIG. 10F is an image of a slice of a nugget isolated from Illustration2. Note the internal voids, carbon structures and nucleation sites (thepocket in the lower left quadrant along the nugget boundary).

FIG. 10G illustrates the growth of rows or layers from a center. Growthcan emanate from a center, for example, resembling a rose, sphere orsimilar recursive structure. The elemental metal macrostructuresproduced from quantum printing, therefore, can be further characterizedby a central domain surrounded by alternating nanolayers of carbon andelemental metal. For example, the carbon and elemental metal nanolayerscan independently be less than about 20 nm in thickness, such as lessthan about 10 nm in thickness, for example, less than about 5 nm inthickness. The macrostructure can be characterized by at least about 5elemental metal nanolayers, such as at least about 10 elemental metalnanolayers emanating from an elemental metal center.

The nanostructures can be spherical, as determined by visual inspectionand SEM. An example of spheroid copper nanostructures can be viewed inFIGS. 8A and 8B. The diameters of the nanostructures can be observed tobe less than 5 microns, such as between 50 and 800 nm, such as between100 and 200 nm. Nanostructures having a flake, scale or chip morphologyhave also been observed. Nanostructures characterized by a highly smoothsurface (or, a surface substantially free of rugosity) have beenobserved. Rugosity is a measure of small-scale variations of amplitudein the height of a surface and can be characterized by the ratio of thetrue surface area divided by the geometric surface area. For example, aperfect sphere would have a rugosity of 1. Thus, nanostructures of theinvention where the rugosity of each structure, as visually observed bySTEM or TEM, is less than about 2, preferably less than about 1.5 suchas less than about 1.2.

In addition, nanostructures of the invention can be characterized by anunusually high roundness. Roundness is used herein to define the ratioof the averaged radius of curvature of the convex regions to acircumscribed circle of the particle (or a surface defined by at least40% of the visible perimeter of the particle, in the case of anellipsoid), as visually observed by STEM, SEM or TEM.

${Roundness} = \frac{\sum\limits_{i = 1}^{n}\left( \frac{r_{i}}{R} \right)}{n}$

Wherein R is the radius of a circumscribed circle, r_(i) is the radiusan inscribed circle at a convex corner i and n is the number ofinscribed circles measured. A roundness of 1 indicates the inscribedcircle overlays the circumscribed circle. The invention includesnanostructures having a roundness of at least about 0.3, preferably atleast about 0.4, 0.5, 0.6, 0.7, 0.8 or 0.9 as visually observed STEM,SEM or TEM.

The following table provides the reproducibility of the experimentation.

#Runs Percent Max Element #Runs (>5σ) (>5σ) (ppm) Nanosphere FormationNi 66 47 70% 14,000 Nanosphere Growth/ Si 66 55 80% 17,000 GerminationElements Ta 42 10 25% 80 Mo 65 13 25% 17 Rh, Pd, 5 N/A — 1.4, 6.2, Pt0.9 N/A: In some instances, Sc 152 N/A — 35 the element was a Y 179 N/A— 7.4 non-detect in the starting Ce 258 48 18% 12 material, confoundingPr 63 N/A — 4.6 statistical comparisons Nd 98 N/A — 36 Sm 39 N/A — 0.59Gd 29 N/A — 0.39 Tb 7 N/A — 5.2 Dy 19 N/A — 0.29 Er 17 N/A — 17 Yb 10N/A — 1.8

The elemental metal nanostructures of the invention can further compriseinternal voids and nanopores. FIG. 13A provides an excellent image ofinternal voids typical of the elemental metal nanostructures of theinvention. Agglomerated nanostructures can be seen. These nanostructureshave apparent diameters or characteristic dimension of less than 1micron. Within the nanostructures, can be seen nanopores with apparentpore diameters of less than about 0.1 micron. Thus, the inventionincludes elemental metal porous nanostructures characterized by anumerical average diameter of less than about 10 μm, preferably lessthan about 1 micron and a numerical average pore diameter of less thanabout 1 μm, such as less than about 500 nm, less than about 200 nm orless than about 100 nm, as calculated visually from an TEM image of anelemental metal macrostructure.

The nanostructures further agglomerate or aggregate to formmacrostructures within the carbon powder. Macrostructures are definedherein to include agglomerates or aggregates of nanostructures as wellas structures visible to the naked human eye. The macrostructures canhave a variety of morphologies, including a nanowire or thread having awidth of less than about 1 micron, as shown in FIG. 8A. FIG. 8Billustrates a nanowire with branching. A nanowire is defined herein toinclude a linear agglomeration of nanostructures characterized by anaspect ratio of at least about 5, such as at least about 10, preferablyat least about 25. Aspect ratio is the ratio of the length to thediameter of the nanowire as determined by visual inspection with an SEM.See FIG. 8C.

Macrostructures characterized by coiled nanostructures have also beenobserved. For example, FIG. 8D illustrates one such coil on the lefthand side of a copper macrostructure made in accordance with theinvention.

Large macrostructures that have also been observed. For example, thelarger particle in FIG. 9A is approximately 1.6 millimeters in lengthand has the appearance of a nugget. This particle is visible to thenaked eye. FIG. 9D is a copper-containing nanowire of larger dimensions,with a length of about 400 microns. In contrast to the threads describedabove, this macrostructure has a hollow or annular appearance. FIGS. 13Band 13C illustrate internal voids typical of elemental metalmacrostructures of the invention from a product of Illustration 1. FIG.13B shows an internal void, or micropore, about 10 microns in diameter.Without being bound by theory, it is believed that such micropores,whether located internally or on the surface of the macrostructure, canbe used as further nucleation sites in the present method for additionalinstantiation. For example, Illustration 1 resulted in a metalmacrostructure characterized by an elemental nanostructure protrudingfrom such a micropore. Thus, the invention includes elementalmacrostructures characterized by at least one micropore protrudingtherefrom an elemental metal nanostructure wherein the nanostructure hasa different metal composition than the macrostructure. FIG. 13Cillustrates an internal fissure characterized by a length of at leastabout 20 nm and width of at least about 5 nm and an aspect ratio of atleast 4. FIG. 13D illustrates the macrostructure which has theappearance of a thick wire or rod. This macrostructure is characterizedby a length of at least about 1 mm and a diameter of at least about 100microns. This macrostructure is preponderantly copper. While thisrepresents a single scan at a single point, more than 50 scans weretaken along the length and cross section of this macrostructure withsimilar results. Tungsten, molybdenum, platinum, silicon and neodymiumwere detected.

FIG. 12 illustrates a silicon microsphere. Elemental analysis suggeststhat the microsphere is a preponderance of silicon dioxide. A rectanglewas removed from the surface of the microsphere, exposing aggregatednanospheres. Iron, aluminum, and sodium were also detected. Similarmetal matrix spheres have been observed containing elementalnanospheres.

As discussed above, macrostructures can be agglomerated nanostructures.The nanostructures can comprise the same or different elements.Typically, detection methods observe the nanostructures can beindividually substantially pure.

The nanoporous carbon compositions described herein and made accordingto the present invention can be used as catalysts and electrodes. Theelemental metal macrostructures described herein can be isolated fromthe nanoporous carbon compositions. For example, sieving the carbonpowder with a porous sieve that will capture metal nanostructures of thedesired size can be beneficial. The elemental metal macrostructures canbe used, for example, in processes typical of mined metals.

Platinum and Other Precious Metal Deposits

Nanoporous carbon compositions and elemental metal macrostructures havebeen isolated that detect precious metals, such as gold and silver, andplatinum group metals, such as platinum, palladium, osmium, rhodium,iridinium and ruthenium. Thus, the invention includes elementalmacrostructures and nanostructures that comprise precious metals, suchas gold and silver, and platinum group metals, such as platinum,palladium, osmium, rhodium, iridinium and ruthenium. The macrostructurescomprising one or more of these elements can have internal carbon, suchas amorphous or sp² carbon, as discussed in more detail above.

Macrostructures can preferably comprise at least 500 ppm platinum, suchas at least about 1000 ppm platinum, preferably at least 10,000 ppmplatinum. Such a macrostructure was made using the GSA protocol, using aZ carbon starting material, a CuG reactor, and nitrogen gas (see,Illustration 2) and with the Electromagnetic Light Combing protocol,using a PEEK carbon starting material, a GG graphite reactor and CO gas(see Illustration 1 substituting CO for helium).

Carbon compositions can preferably comprise platinum nanostructureshaving a concentration of at least about 500 ppb platinum, such as atleast about 1000 ppb, preferably at least about 10,000 ppb platinum.Such carbon compositions were made using the GSA protocol, helium gas,the GPtIr reactor, which lines the cup with a platinum foil and avariety of nanoporous carbon starting materials.

The target metal (e.g., precious metals, such as gold and silver, andplatinum group metals, such as platinum, palladium, osmium, rhodium,iridinium and ruthenium) can be extracted from the carbon compositionand other metals in the macrostructure by methods routinely used in themining industry.

Four illustrations, representative of platinum containing compositions,with third party characterizations, are set forth in the followingtable:

Sample Example Example Example Example Number 2 12 9 50 Illustration No.2 1 1 6 Experimental GSA E/LC E/LC QPP Protocol Rx Assembly CuG GGG_(g)F CuG Gas N₂ Co Kr He-H₂ Composition Carbon Type Z-Lot APK-800APKI-108 MSP- 20X Temperature, 180° C. 450° C. 450° C. 25° C. T_(ops)Elements (Instantiated) Category-1 1 1 2 1 Elements Cu Cu Fe, Cr FeCategory-2 3 3 6 7 Elements Na, Sl, W, Al, Ni, Na, Ca, Ca, Re Zn, Hf, V,Cr, Pt Pb, Bi Mn, Ni, Cu Category-3 5 14 8 5 Elements Al, Si, Na, Al,Si, Ca, Zn, Zr, K, K, Ca, Mn, Cu, Mo, Sn, Fe, Ag Ti, Cr, Mo, Sn, Sb Fe,Ni, Sb, W Mo, Sn, Ba, Ta, Os, Pb Category-4 46 46 33 18 Elements Be, B,Li, Be, B, Li, B, Na, Ti, Co Mg, P, Mg, P, Mg, P, Sc, Ti, Sc, V, K, Sc,Ti, V, Cr, Mn, Co, V, Co, Mn, Co, Zn, Ga, Ga, Ge, Se Ni, Zn, Ge, Se Ga,Ge, As, Se, Rb, Sr, Rb, Sr, Rb, Sr, Y, Nb Y, Zr, Y, Zr, Zr, Nb, Nb, Mo,Nb, Ru, Ru, Pb, Ru, Ag, Cd, Ag, Cd, Cd, Sn, Sb, Te Te Sb, Te, Cs, Ba,La, Ce, Ba, Ce, Ce, Pr, La, Nd, Pr, Nd, Nd, Gd, Nd, Sm, Sm, Gd, Sm, Eu,Yb Eu, Gd, Eu Gd, Tb, Tb, Dy, Dy, Ho, Ho, Er, Er, Tm, Tm. Yb, Yb, Lu LuHf, W, Hf, Ir, Re, Os, Hf, W Re, Os, Pt, Au, Pt, Hg, Ir, Au, Hg, Tl, TlHg, Tl, Bi, Th, Pb, Bi, U Th, U Instantiated Elements 55 64 49 31Analysis Internal ED-XRF, ED-XRF, ED-XRF, ED-XRF, EBD- EBD- EBD- EBD-SEM, SEM, SEM, SEM, optical optical optical optical micro- micro- micro-micro- scopy scopy scopy scopy External LA-ICP- LA-ICP- LA-ICP- LA-ICP-MS, MS, MS, MS, EBD- EBD- EBD- EBD- SEM, SEM, SEM, SEM, optical opticaloptical optical TEM, CAMECA TEM, STEM, SX5 STEM, SEM, Electron SEM, EELSMicro- Gamma probe Spectro- scopy

Methods and Apparatus

Conceptually, the apparatus for baseline experimentation can be brokeninto two primary areas: Gas Processing and Reactor Assembly.

Gas Processing:

The gas processing section controls gas composition and flow rate, withthe optional embedding of electromagnetic (e.g. light) information orelectromagnetic gas pre-treatment to the reactor. The invention includesan electromagnetic embedding enclosure (E/MEE or EMEE), or apparatus,for processing a gas comprising or consisting of:

-   -   a central processing unit and power supply;    -   one or more gas supplies;    -   a housing having a housing inlet and housing outlet;    -   an upstream gas line that is in fluid connection with each gas        supply and the housing inlet;    -   an internal gas line in fluid connection with the housing inlet        and housing outlet;    -   a downstream gas line in fluid connection with the housing        outlet;    -   at least one pencil lamp positioned below the internal gas line,        at least one pencil lamp positioned above the internal gas line        and/or at least one pencil lamp positioned to the side of the        internal gas line;    -   a short wave lamp and/or a long wave lamp; and    -   an optional coil wrapped around the internal gas line, operably        connected to a frequency generator;    -   wherein each lamp is independently rotatably mounted, located        along the length of the internal gas line, and powered by the        power supply; and    -   wherein the central processing unit independently controls        powering the frequency generator, if present, and each lamp and        the rotation position of each lamp.

Feed gases can preferably be research grade or high purity gases, forexample, as delivered via one or more gas supplies, such as a compressedgas cylinder. Examples of gases that can be used include, for example,air, oxygen, nitrogen, hydrogen, helium, neon, argon, krypton, xenon,ammonium, carbon monoxide, carbon dioxide and mixtures thereof.Preferred gases include nitrogen, helium, argon, carbon monoxide, carbondioxide and mixtures thereof. Nitrogen and helium are preferred. Thegases can be free of metal salts and vaporized metals.

One or more gases (e.g., 2, 3, 4, 5, or more gases) can optionally passthrough a gas manifold comprising mass flow meters to produce a gascomposition, also called the reactor feed gas. The reactor feed gas maythen either by-pass an electromagnetic (EM) embedding enclosure (E/MEE)or pass through one or more E/MEEs. The E/MEE exposes the reactor feedgas to various electromagnetic field (EMF) sources. Flow rates,compositions, and residence times can be controlled. The rate of flow ofthe reactor feed gas can be between 0.01 standard liters per minute(SLPM) and 10 SLPM, or 100 SLPM or more. A constant flow of gas canmaintain a purged environment within the reactor. The schematics shownin FIG. 1 depicts a flow path for the gases through a sample E/MEE. Thesample E/MEE comprises a series of lights and coils that can optionallyexpose the reactor feed gas to EM radiation. EMF sources within theE/MEE can be energized simultaneously or in sequence or a combinationthereof.

FIG. 1 is an illustration of an E/MEE of the invention. Gas enters theE/MEE via the inlet 101, or entrance, in line 102 and exits at theoutlet, or exit, 110. The inlet 101 and outlet 110 may optionally havevalves.

Line 102 can be made of a transparent or translucent material (glass ispreferred) and/or an opaque or non-translucent material, such asstainless steel or non-translucent plastic (such as TYGON® manufacturedby Saint-Globain Performance Plastics) or a combination thereof. Usingan opaque material can reduce or eliminate electromagnetic exposure tothe gas as the gas resides within the line. The length of line 102 canbe between 50 cm and 5 meters or longer. The inner diameter of line 102can be between 2 mm and 25 cm or more. Line 102 can be supported onand/or enclosed within a housing or substrate 111, such as one or moreplates, with one or more supports 112. For example, substrate 111 can beconfigured as a plane or floor, pipe or box. Where the substrate is abox, the box can be characterized by a floor, a ceiling and side walls.The box can be closed to and/or insulated from ambient EM radiation,such as ambient light.

One or more lamps (such as 2, 3, 4, 5, 6, 7, 8, 9, 10 lamps or more) canbe configured within the E/MEE. Lamps (numbered individually) arepreferably pencil lamps characterized by an elongated tube with alongitudinal axis. The pencil lamps can independently be placed suchthat its longitudinal axis is (i) parallel to the line 102, (ii)disposed radially in a vertical plane to the line 102, or (iii)perpendicular to the plane created along the longitudinal axis of theline 102 or along the vertical axis of the line 102.

Each lamp can, independently, be fixed in its orientation by a support112. Each lamp can, independently, be affixed to a pivot 113 to permitrotation from a first position. For example, the lamps can be rotatedbetween about 0 and 360 degrees, such as about 45, 90, 135, 180, 225 or270 degrees, preferably about 90 degrees relative to a first position.The rotation can be with respect to the x, y, and/or z axis wherein (i)the x-axis is defined as the axis parallel to the gas line and itsvertical plane, (ii) the y-axis defining the axis perpendicular to thegas line and parallel to its horizontal plane, and (iii) the z-axis isdefined as the axis perpendicular to the gas line and parallel to itsvertical plane.

Referring to the specific pencil lamps within an E/MEE, line 102 isconfigured along the E/MEE with gas flowing from the inlet 101 andexiting at the outlet 110. Lamp 103, a neon lamp, is first and is shownabove line 102 oriented to be along the z-axis and perpendicular to line102, with the tip of the lamp pointed towards line 102. Lamp 109, akrypton lamp, is shown below line 102 oriented to be parallel to thex-axis, with the tip pointing towards the outlet 110. Lamps 104 and 105,a long wave and short wave lamp, respectively, are shown parallel toline 102 oriented to be along the x-axis with the tips pointing towardsthe inlet. Lamp 122, an argon lamp, is shown to be below line 102oriented to be parallel to the x-axis, with the tip pointing towards theinlet 101 at approximately the same distance from the inlet as lamps 104and 105. Lamp 106, a neon lamp, is downstream at about the midpoint ofthe E/MEE, is above line 102 with the tip pointing down. Lamp 107, axenon lamp, is shown downstream of lamp 106 above line 102, parallel tothe x axis of line 102 and points toward the outlet 110. Lamp 108, anargon lamp, is below line 102 and the tip is pointing toward line 102along the z-axis. Optional coil 120 is wrapped around line 102. Each ofthese lamps can be independently rotated, for example, 90 degrees alongany axis. Each lamp is connected to a power supply or power source toturn on or off the power. Each lamp can be independently rotated 1, 2,3, 4 or more times during the process. For convenience, each lamp isheld by a pivot that can be controlled by a central processing unit,such as a computer programmed to rotate the pivot and provide power toeach lamp. For the ease of describing the experimental procedures, eachorientation of each lamp is called “position n” wherein n is 0, 1, 2, 3,4, or more. As the procedure is conducted, each lamp can be powered forspecific periods of time at specific amperage(s) and positioned orrepositioned.

In the exemplification described below, the initial bulb position foreach lamp is described with a degree. A zero degree (0°) reference pointis taken as the 12 o'clock position on the glass pipe when looking downthe gas pipe in the direction of intended gas flow (e.g., when lookingat the E/MEE exit). The length of the glass pipe or line is taken as theoptical length (e.g., in this instance 39 inches). For example, 6 inchesfrom the end is defined as 6 inches from the optical end of pipe.

The lamps can be placed above, below, or to the side (for example, levelwith the longitudinal axis or a plane parallel to (above or below) thelongitudinal axis), for example, of line 102. The lamps can beindependently placed between 5 and 100 cm from the center of the line102 in the vertical plane, as measured from the tip of the lamp to thecenter of line 102. One or more lamps can be placed in the same verticalplane along line 102, as illustrated by lamps 122, 104, and 105. Twolamps are in the same vertical plane if they (as defined by the tip orbase of the lamp) are the same distance from the inlet 101. Preferably,lamp 105 can be placed in a plurality of (e.g., 2, 3, 4, 5 or more)vertical planes along the length of line 102 within the E/MEE. Further,one or more lamps can be placed in the same horizontal plane above,below or through line 102, as shown with lamps 104 and 105. Two lampsare in the same horizontal plane if they (as defined by the tip or baseof the lamp) are the same distance from the center of line 102.Preferably, lamps can be placed in a plurality of (e.g., 2, 3, 4, 5 ormore) horizontal planes along the length of line 102 within the E/MEE,as generally illustrated.

It is understood that “pencil lamps,” as used herein, are lamps filledwith gases or vapor that emit specific, calibrated wavelengths uponexcitation of the vapor. For example, pencil lamps include argon, neon,xenon, and mercury lamps. For example, one or a plurality of lamps canbe selected from argon, neon, xenon or mercury or a combination thereof.Preferably, at least one lamp from each of argon, neon, xenon andmercury are selected. Wavelengths between 150 nm and 1000 nm can beselected. One example of a pencil lamp is a lamp characterized by anelongated tube having a tip and a base.

Long wave and/or short wave ultraviolet lamps can also be used. Pencillamps used in the E/MEE were purchased from VWR™ under the name UVPPen_Ray® rare gas lamps, or Analytik Jena in the case of the UV shortwave lamps.

A power supply is operably connected to independently to each lamp,E/MEE coil, and frequency generator. The power supply can be AC and/orDC.

The E/MEE can be open or enclosed. Where the E/MEE is enclosed, theenclosure is typically opaque and protects the gas from ambient light.The enclosure can be made of a plastic or resin or metal. It can berectangular or cylindrical. Preferably, the enclosure is characterizedby a floor support.

In baseline experimentation the gases by-pass the E/MEE section and arefed directly to the reactor assembly. The energy levels and frequenciesprovided by the EM sources can vary.

FIG. 4A provides a second illustration of an E/MEE of the invention. Gasenters the E/MEE at inlet 401 and exits at outlet 409 along line 410.Pencil lamp 402 and Pencil lamp 403 are shown parallel to and above line410 along the vertical plane through line 410 axis. Pencil lamps 404 and405 are parallel to and below line 410 in the same horizontal planeequidistant from the vertical plane through line 410. Pencil lamp 406 isshown above and perpendicular to line 410, positioned along the z axis.An optional coil 407 is a conductive coil wrapped around line 410.Pencil lamp 408 is shown below and perpendicular to line 410 along the yaxis. Substrate 411 provides a base for supports 412. Pivots 413 controlthe position of each pencil lamp and permit rotation along axis x, y andz. An optional x-ray source 429 is also shown directed towards the coil407.

The coil 407 is preferably made of conducting material and is connectedto a power supply and, optionally, a frequency generator. The coil cancomprise copper, aluminum, platinum, silver, rhodium, palladium or othermetals or alloys (including braidings, platings and coatings) and canoptionally be covered with an insulating coating, such as glyptal. Itcan be advantageous to use a braid of 1, 2, 3 or more metal wires. Thecoil can be manufactured from wire typically used in an induction coiland can vary in size and the number of turns. For example, the coil cancomprise, 3, 4, 5, 6, 7, 8, 9, 10 or more turns. The inner diameter ofthe coil can be between 2 cm and 6 cm or more and preferably snugly fitsthe line 410. The wire used can have a diameter of between 5 mm and 2cm.

An x-ray source 429 can included in the E/MEE. For example, the x-raysource can be directed at line 410 along the line between the inlet 401and outlet 409. For example, it can be advantageous to direct the x-raysource at coil 407, where present.

Reactor Assembly (RA):

The invention further relates to a reactor assembly comprising:

-   -   A gas inlet and one or more gas outlets;    -   A reactor chamber, preferably containing a nanoporous carbon        material;    -   A first porous fit defining a floor of the reactor chamber,    -   A second porous frit defining the ceiling of the reactor        chamber; wherein each porous frit has a porosity that is        sufficient to allow a gas to permeate into the reactor chamber        and contain a nanoporous carbon material;    -   An optional reactor cup defining side walls of the reactor        chamber;    -   A reactor cap positioned above the second porous frit;    -   A reactor body disposed below the first porous frit;    -   A reactor head space disposed above the reactor cap;    -   An optional foil disposed between the reactor chamber and        reactor cup;    -   A plurality of coils surrounding the reactor body and/or the        reactor chamber operably connected to a power supply and        frequency generator;    -   An optional x-ray source configured to expose the reactor head        space to x-rays;    -   One or more optional lasers configured to direct a laser towards        a frit and/or through the reactor chamber;    -   A computer processing unit configured to control the power        supply, frequency generator and the optional x-ray source and        lasers.

The invention also includes a reactor assembly comprising:

-   -   A gas inlet and one or more gas outlets;    -   A reactor chamber, preferably containing a nanoporous carbon        material;    -   A first porous frit defining a floor of the reactor chamber,    -   A second porous frit defining the ceiling of the reactor        chamber; wherein each porous frit has a porosity that is        sufficient to allow a gas to permeate into the reactor chamber        and contain a nanoporous carbon material;    -   A reactor head space disposed above the reactor cap;    -   2, 3, 4, 5 or more RA coils surrounding the reactor chamber        and/or reactor head space operably connected to an RA frequency        generator and power supply;    -   2, 3, 4, 5 or more pairs of lamps wherein the pairs of lamps are        disposed circumferentially around the RA coils and define a        space between the pairs of lamps and the RA coils;    -   An optional x-ray source configured to expose the reactor        chamber to x-rays;    -   One or more optional lasers configured to direct a laser through        the reactor chamber; and    -   A computer processing unit configured to control the power        supply, frequency generator and the optional x-ray source and        lasers.

As shown in FIGS. 2A and 2B, the reactor assembly comprises a reactorbody 202 and starting, or charge, material 204 (which is generally ananoporous carbon powder) and is located downstream of the gas sources221 and E/MEE 222, as shown in FIG. 2A. As described above, it ispossible for reactor feed gas to bypass the E/MEE. The reactor body 202can be a packed bed tubular micro-reactor surrounded by one or moreconducting coils 208, as illustrated in FIG. 2B, a cross section of thereactor assembly.

The conducting coil 208 can be manufactured from electrically conductingmaterial, such as copper, aluminum, platinum, silver, rhodium, palladiumor other metals or alloys (including braidings, platings and coatings)and can optionally be covered with an insulating coating, such asglyptal. The coil can be manufactured from wire typically used in aninduction coil and can vary in size and the number of turns. Forexample, the coil can comprise, 3, 4, 5, 6, 7, 8, 9, 10 or more turns.The inner diameter of the coil can be between 2 cm and 6 cm or more andpreferably snugly fits the reactor body containment 207. The wire usedcan have a diameter of between 5 mm and 2 cm.

Each conducting coil 208 (or coil) can generate inductive heat and,optionally, a magnetic field. Standard induction coils or reverse fieldinduction coils (coils that have a lower and upper sections connectedthrough an extended arm that allows the sections to be wound in oppositedirections, thereby producing opposing magnetic fields) are preferred.The coil 208 can be water-cooled via a heat exchanger. The coil can beconnected to a power flange 210, which can be water cooled as well andin turn can connect to a power supply, such as an Ambrell 10 kW 150-400kHz power supply. In baseline experimentation a standard coil was usedwith simple copper windings. The windings can form a coil such that theconnection to the power supply is at opposite ends of the coil FIG. 5Aor the coil can return such that the connection to the power supply areadjacent, as shown in FIG. 5B.

The reactor assembly can optionally further comprise one or more coils208, preferably surrounding the reactor body and its containment system.For example, the reactor assembly can comprise 1, 2, 3, 4, 5, 6, 7, 8,9, or 10 or more coils, also called RA coils. As shown in FIG. 2B, oneor more electromagnetic (E/M) coils can be used to provide magneticfields. Preferably, 1, 2, 3, 4, or 5 or more E/M coils can be used, morepreferably 3, 4, or 5 E/M coils. FIG. 3 shows groupings of three coils,for example, which can generally be numbered 1, 2, or 3, from top tobottom. A grouping of coils, as shown in FIG. 3A-3E, can be called aboundary. Where a plurality of groupings is used, the number of coilsused is independently selected. Further, the groupings can beequidistantly spaced along or irregularly spaced.

Coils can be manufactured from electrically conducting materials, suchas copper, platinum, silver, rhodium, palladium and, wire braids orcoated wires of two or more materials. Each coil in a grouping may bemade of the same material or different. For example, a grouping can bemade such that each coil is made of a different material. For example, abraiding of copper wire and silver wire can be used. Silver platedcopper wire can be used. A first RA coil can be made of a copperwinding. A second RA coil can be a copper/silver braid. A third RA coilcan be a platinum wire winding. An RA coil can be configured to create amagnetic field and wherein each power supply independently provides ACand/or DC current. Any one or all RA coils can be optionally lacquered.

The coils are preferably circular in geometry. However, othergeometries, such as rounded shapes, ellipses and ovoids can be used. Thewire diameter can be between about 0.05 mm (>about 40 gauge) and about15 mm (about 0000 gauge) or more. For example, the wire diameter can bebetween about 0.08 mm (about 40 gauge) and about 0.8 mm (about 20 gauge)wire. Excellent results have been obtained using 0.13 mm (36 gauge)wire. Coils can be wire windings (e.g., the wire can be wound in 1, 2,3, 4, 5, 6, 7, 8, 9, 20, or more turns or can be a single turn. When thecoil is made with a single winding, the diameter or width of the wirecan preferably be 10 mm or more in diameter. In this context, a “wire”can also be considered a band where the width of the material is greaterthan the depth. FIG. 3 provides illustrations or views of various coilsand groupings of coils. A wire coil can be made of a single wire, a wirealloy or two or more wires. For example, two wires comprising differentmetals can be wound or braided together.

The inner diameter (or dimension(s) where the coil is not a circle) ofeach coil can be the same or different and can be between 2 and 200 cm.

Coils 208 can independently be connected to one or more power supplies,such as an AC or DC power supply or combination thereof. For example, anAC current can be supplied to alternating (1, 3, and 5, for example) oradjacent coils (1, 2 and/or 4, 5, for example) while DC current issupplied to the remaining coils. Current can be provided (independently)in a frequency, such as in a patterned frequency, e.g., triangle, squareor sine pattern or combination thereof. The frequency supplied to eachcoil can be the same or different and between 0 to 50 MHz or higher.While the coils 208 can generate and transfer thermal energy, or heat,to the reactor feed gas they are predominantly used to create a magneticfield.

The power supply can be an AC and/or DC power supply or combinationthereof. Current can be provided (independently) in a frequency, such asin a patterned frequency, e.g., triangle, square or sine pattern orcombination thereof. The frequency supplied to each coil can be the sameor different and between 0 to 50 MHz or higher, such as between 1 Hz to50 Mhz.

As described above, the RA coils typically surround the reactor chamberand/or reactor head space. For example, a first RA coil can be alignedwith the first (or bottom) frit. A second RA coil can be aligned withthe reactor chamber or nanoporous carbon bed. A third RA coil can bealigned with the second (or top) frit. Where present, a fourth RA coilcan be disposed between the first RA and the second RA coil. Whenpresent, a fifth RA coil can be disposed between the second RA coil andthird RA coil. When two or more reactor chambers, or nanoporous carbonbeds are present, it can be desirable to add additional RA coils, alsoaligned with a second or additional reactor chambers or nanoporouscarbon beds. Additional RA coils can be added to align with additionalfrits, when present.

The RA coils can typically be supported in a support or stator tomaintain a fixed distance between each coil. The support, when present,can be transparent. In one embodiment, the RA coils can be configured ina cartridge that can be removed or moved.

The RA coils can, additionally or alternatively, be aligned with thereactor headspace. The reactor headspace can typically be a volume abovethe second, or top, frit. It is understood that where the reactorassembly is positioned horizontally (or at some other angle thanvertical), the geometry of the spaces is maintained, albeit rotated. Thereactor headspace can typically be an enclosed volume. For example, thereactor assembly can be inserted into a closed ended transparent (e.g.,glass) tube, vial or bottle. The reactor assembly can be movably engagedwith the RA coils (or boundary), thereby permitting each RA coil toalign to a different element within the reactor assembly. For example,the first RA coil can be realigned with the reactor chamber.

Reactor body 202 can also be a packed, moving or fluidized bed or otherconfiguration characterized by one or more chambers that receive thecharge material 204 and facilitates transfer of a reactor feed gasthrough the charge material 204 and can transfer thermal and/orelectromagnetic energy to the charge material 204. The reactor body 202is generally contained within a housing, e.g., closed end tube, 207 andfrits 203, which function to contain the charge material 204. It can beadvantageous to use a reactor within a translucent or transparenthousing, such as quartz or other materials characterized by a highmelting point. The volume of the reactor bed can be fixed or adjustable.For example, the reactor bed can contain about 1 gram, or less ofstarting material, between about 1 g to 1 kg of starting material ormore. Where the reactor assembly comprises two or more reactor chambers,the reactor chambers are preferably directly or indirectly stacked,preferably having a common central axis and can be separated by one ortwo frits.

The reactor body 202 can be made of a thermally conductive material,such as graphite, copper, aluminum, nickel, molybdenum, platinum,iridium, cobalt, or niobium, or non-thermally conducting material, suchas quartz, plastic (e.g., acrylic), or combinations thereof. An optionalcup 206 capped with cap 205 can be advantageous. The cup and capmaterial can be independently selected. For example, a graphite cup canbe combined with a graphite cap. A copper cup can be combined with agraphite cap. A graphite cup can be combined with a copper cap. A coppercup can be combined with a copper cap and so on.

The reactor assembly can also receive the gas line through the entrance,or inlet, 201 and to provide an exhaust through an exit, or outlet, 209,optionally controlled by valves. A head space defined by a closed endtube 207 can be configured above the reactor body. The reactor body ispreferably made of graphite, copper, or other inorganic rigid material.The gas line is preferably made of an inert tubing, such as glass,acrylic, polyurethane, plexiglass, silicone, stainless steel, and thelike can also be used. Tubing can, optionally, be flexible or rigid,translucent or opaque. The inlet is generally below the charge material.The outlet can be below, above or both.

Frits 203 used to define the chamber containing the charge material arealso shown. The frits can be made of a porous material which permits gasflow. The frits will preferably have a maximum pore size that is smallerthan the particle size of the starting material. Pore sizes of between 2and 50 microns, preferably between 4 and 15 microns can be used. Thethickness of the frits can range satisfactorily between 1 and 10 mm ormore. The frits are preferably made of an inert material, such as silicaor quartz. Porous frits from Technical Glass Products (Painesville Tp.,Ohio) are satisfactory. On the examples below, fused quartz #3 porousfrits (QPD10-3) with a pore size between 4 and 15 microns and athickness of 2-3 microns and fused quartz frits with a pore size between14 and 40 microns (QPD10-3) were used. The purity of the fritsexemplified herein was very high, 99.99% wt, to ensure that the resultsobtained cannot be dismissed as the result of contamination. Frits oflower purity and quality can also be used. The diameter of the porousfrit is preferably selected to permit a snug fit within the reactorinterior, or cup. That is, the diameter of the porous frit isapproximately the same as the inner diameter of the reactor or cup, ifpresent.

Referring to FIGS. 6A and 6B, a foil can optionally encase the chambercontaining the charge material on the inside and/or outside of the fritsand/or cup, thereby creating a metal boundary surrounding the startingmaterial. The foil can be a metal, such as copper, platinum, niobium,cobalt, gold, silver, or alloys thereof. The foil can also be graphiteor the like. The foil can be between 0 and 0.5 cm thick, preferably 1-10mm. The profile of the reactor can be linear or it can be configured tocontain a constriction below the lower frit, providing the generalappearance of a lollipop. The gas line 102 is also shown.

The reactor chamber is sized to contain the desired amount of chargematerial 204. For the experiments described herein, the chamber isdesigned to contain between 20 mg to 100 grams of nanoporous carbonpowder. Larger reactors can be scaled up.

The reactor assembly may be augmented with additional forms ofelectromagnetic radiation, such as light. FIG. 4B exemplifies lightsources 426 and 427 that generate light directed through the reactorhousing 415 and starting material contained therein. Preferred lightsources 426 and 427 can be lasers and/or can emit light in a wavelengthbetween 10 nm and 1 mm. The light is optionally subjected to one or morefilters 428, as shown in the use of light sources (beams) in FIG. 4B.Preferably, the reactor assembly comprises 2, 3, 4, 5 or more pairs oflamps disposed circumferentially around the RA coils. Pencil lamps, suchas the lamps used within the E/MEE which is incorporated herein byreference from above, are preferred. The pairs of lamps preferablydefine a boundary surrounding the coil and are not touching or otherwiseadjacent to the coils. Two lamps are considered paired where they areproximal to each other, such as within the same plane with the centeraxis of an RA coil. Paired lamps can be parallel or orthogonal to eachother and the RA coil center axis. Lamps can be considered proximal toeach other if the space between any two points between the lamp tip andbase is within 10 cm, preferably within 5 cm. Lamps that are positionedorthogonally to the RA coil center axis are generally positioned alongthe line defined by the radius of one or more RA coils.

The RA lamps, e.g., the pencil lamps proximal to the reactor body, canbe matched, or paired, to one or more E/MEE lamps, e.g., the pencillamps residing within the E/MEE housing and proximal to the gas line.For example, where an E/MEE pencil lamp is a neon lamp, a pair of RAlamps can be neon pencil lamps. Additionally, where an E/MEE pencil lampis a neon lamp, a pair of RA lamps can be neon pencil lamps. Suchmatched lamps can emit light characterized by substantially the samewavelength. This can be conveniently achieved by using lamps from thesame manufacturer with the same specifications.

The reactor can be in a closed or open housing 415 and can be supportedtherein by reactor supports. The reactor feed gas is directed to thereactor inlet frit, or bottom frit, directed through the startingmaterial contained within the housing 415 and exits the reactor at thereactor exit frit, or top frit. The reactor feed gas can then beexhausted or recycled, optionally returning to the E/MEE for furthertreatment.

The reactor can further comprise an x-ray source 211 (FIG. 2C) or 424(FIG. 4B) and/or one or more lasers 212 (FIG. 2C) or 426 and 427 (FIG.4B). Preferred x-ray sources include a mini-x. The x-ray is preferablydirected through the reactor towards a gas headspace, or target holder213, above the charge material. The x-ray can be directly or indirectlyprovided from the source, such as by reflecting the x-ray from a foildisposed above or below a frit.

FIG. 15A illustrates a top view of a preferred reactor assembly. Pencillamp 1501, pencil lamp 1502 and pencil lamp 1503 are shown with the tipdirected towards a center axis of the reactor assembly along a radius ofthe reactor assembly. Pencil lamp 1504, pencil lamp 1505 and pencil lamp1506 are shown directed parallel to a center axis of the reactorassembly and are disposed in a plane along a radius of the reactorassembly. Pencil lamp 1501, together with pencil lamp 1504, form a firstRA lamp pair. Pencil lamp 1502, together with pencil lamp 1505, form asecond RA lamp pair. Pencil lamp 1503, together with pencil lamp 1506,form a third RA lamp pair. As with the E/MEE pencil lamps, each RA lampcan be rotated along its x, y or z axis. Each pair can optionally residewithin the same radial plane, as shown. Outer support 15109 providessupport for the pencil lamps 1501, 1502 and 1503. Inner support 15110provides support for the pencil lamps 1504, 1505 and 1506. The outer andinner supports are preferably made of non-conductive materials (such aspolymers or resins) and are preferably transparent. An optional x-raysource 1507 is shown directing x-rays towards the center axis of thereaction chamber 1508. Reactor connector 15111 is also shown.

FIG. 15B is a perspective view of this reactor assembly. Pencil lamp1509, pencil lamp 1510 and pencil lamp 1511 are shown directed with thetip towards a center axis of the reactor assembly along a radius of thereactor assembly. The tip of each lamp aligns with the center, or third,RA coil 1517 and is in the same horizontal plane. Pencil lamp 1512,pencil lamp 1513 and pencil lamp 1514 are shown directed parallel to acenter axis of the reactor assembly, disposed in a plane along a radiusof the reactor assembly and is characterized by a tip pointing towardstop of the reactor, away from the gas inlet 1520. These lamps areillustrated above the horizontal pencil lamps. The length of each pencillamp align with RA coils 1516, 1517 and 1518. Outer support 15109 andinner support 15110 support the pencil lamps. An optional x-ray source1515 is shown directing x-rays towards the center axis of the reactorassembly above the third RA coil 1516. Disposed within the reactorassembly can be a reflecting plate to direct the x-ray towards thereaction chamber. Reactor connector 15111 is also shown, as well asother non-material connectors and spacers. Gas inlet 1520 and gas outlet1519 are also shown.

FIG. 15C is a second perspective view of a reactor assembly. Pencil lamp1521, pencil lamp 1522 and pencil lamp 1523 are shown directed with thetip towards a center axis of the reactor assembly along a radius of thereactor assembly. Pencil lamp 1524, pencil lamp 1525 and pencil lamp1526 are shown directed parallel to a center axis of the reactorassembly, disposed in a plane along a radius of the reactor assembly andis characterized by a tip pointing towards the bottom of the reactor,towards the gas inlet 1532. These vertical lamps are shown above thehorizontal lamps and, again, each pair of lamps can optionally lie inthe same radial plane. The tip of each pencil lamp aligns with the thirdRA coil 1528. Outer support 15109 and inner support 15110 support thepencil lamps. Three RA coils 1528, 1529 and 1530 are shown. An optionalx-ray source 1527 is shown directing x-rays towards the center axis ofthe reactor assembly. Disposed within the reactor assembly can be areflecting plate to direct the x-ray towards the reaction chamber.Reactor connector 15111 is also shown, as well as other non-materialconnectors and spacers. Gas inlet 1532 and gas outlet 1531 are alsoshown.

FIG. 15D is a cross sectional side view of the reactor assembly,stripped of the pencil lamps and x-ray source. Gas enters at the inlet1541 and exits at the outlet 1540. RA coils 1537, 1538 and 1539 areshown. The first, or bottom, frit 1535 and the second, or top, frit 1533contain the reaction chamber 1534, which can be charged with nanoporouscarbon powder. The reactor body 1536 is also shown. Other non-materialspacers and connectors remain unlabeled.

FIG. 15E is a second cross sectional side view of a reactor assembly,stripped of the pencil lamps and x-ray source. Gas enters at the inlet1551. RA coils 1545, 1546 and 1547 are shown. The first, or bottom, frit1544 and the second, or top, frit 1542 contain the reaction chamber1543, which can be charged with nanoporous carbon powder. The reactorbody 1548 is also shown. X-ray source 1549 directs x-rays towards thecenter axis of the reacto assembly which is then deflected towards thereactor chamber with element 1550. Other non-material spacers andconnectors remain unlabeled.

FIG. 15F is a second cross sectional side view of a reactor assemblywith the pencil lamps and x-ray source. Gas enters at the inlet 1564. RAcoils 1555, 1556 and 1557 are shown. The first, or bottom, frit 1554 andthe second, or top, frit 1552 contain the reaction chamber 1553, whichcan be charged with nanoporous carbon powder. The reactor body 1558 isalso shown. Vertical pencil lamps 1560 and 1561 are shown as arehorizontal pencil lamps 1560 and 1559. X-ray source 1562 directs x-raystowards the center axis of the reacto assembly which is then deflectedtowards the reactor chamber with element 1563. Other non-materialspacers and connectors remain unlabeled.

FIG. 15G is a perspective view of a reactor assembly with the pencillamps and x-ray source. Gas enters at the inlet 1577 and exits at outlet1578. A first laser 1575 and a second laser 1576 directing radiationtowards the reaction chamber along the axis of the reactor assembly isshown. RA coils 1571, 1572 and 1573 are shown. In this embodiment pencillamps 1565, 1566, 1567, 1568, 1569, and 1570 are all shown horizontallydisposed in pairs along the radius towards the reactor assembly centralaxis. Tips are proximal to RA coils 1571, 1572 and 1573. X-ray source1574 directs x-rays towards the center axis of the reactor assembly.Support 15109 supports all of the horizontal pencil lamps. Othernon-material spacers and connectors remain unlabeled.

FIG. 15H is a perspective view of a reactor assembly with the pencillamps and x-ray source. Gas enters at the inlet 1591 and exits at outlet1592. A first laser 1589 and a second laser 1590 directing radiationtowards the reaction chamber along the axis of the reactor assembly isshown. RA coils 1585, 1586 and 1587 are shown. In this embodiment pencillamps 1579, 1580, 1581, 1582, 1583, and 1584 are all shown verticallydisposed in pairs in radial planes aligned with the RA coils. Tips areproximal to RA coils 1585, 1586 and 1587. X-ray source 1588 directsx-rays towards the center axis of the reactor assembly. Supports 15109and 15110 support the pencil lamps. Other non-material spacers andconnectors remain unlabeled.

FIG. 15I is a perspective view of a reactor assembly illustrating 5 RAcoils, horizontal pencil lamps and an x-ray source. Gas enters at theinlet 15107 and exits at outlet 15108. A first laser 15105 and a secondlaser 15106 directing radiation towards the reaction chamber along theaxis of the reactor assembly is shown. RA coils 1599, 15100, 15101,15102 and 15103, defining a cylindrical boundary, are shown. In thisembodiment pencil lamps 1593, 1594, 1595, 1596, 1597, and 1598 are allshown horizontally disposed in pairs in radial planes aligned with theRA coils. Tips are proximal to RA coils 1599 and 15103. X-ray source15104 directs x-rays towards the center axis of the reactor assembly.Support 15109 support the pencil lamps. Other non-material spacers andconnectors remain unlabeled.

Ni-1 Reactor:

Referring to FIG. 17A, the reactor body (1702) is based on a high puritynickel (Ni) rod. The Ni rod, with an outside diameter of 15.873 mm (OD)is bored through then machined with a female thread on one end. Theinside diameter allows for the installation of upper and lower frit andcarbon bed. The carbon reaction medium is housed inside the reactor body(1702). To load the reactor, the reactor body (1702) is positioned withthe gas discharge opening (1706) facing down on a flat surface. A quartzfrit (1705) is placed inside the reactor body (1702) to form the uppercontainment. 100 mg of carbon is then loaded into the reactor body(1702). After loading of the graphite bed inside the reactor body(1702), a second quartz frit (1703) is installed. A reactor pole (1701),machined out of a high purity graphite rod with matched male threads forthe reactor body (1702), is then screwed onto the reactor body (1702).The reactor pole (1701) is designed to provide the identical graphitebed compression as that provided by the cup design (1708).

NiPtG Reactor:

Referring to FIG. 17B, the reactor body (1707) is based on a high puritynickel (Ni) rod. The Ni rod, with an outside diameter of 15.873 mm (OD)is bored through then machined on one end to have an inside diameter of11.68 mm (ID). The inside diameter allows for the installation of agraphite cup (1708) and a 0.025 mm platinum (Pt) foil (1713). Thegraphite cup provides for reactor wall and foil isolation from thecarbon bed. The carbon reaction medium is housed inside a 99.9999 wt %pure graphite cup (1708). To load the reactor, a quartz frit (1709) isplaced inside the graphite cup (1708) to form the bottom containment.100 mg of carbon (1710) is then loaded into the cup (1708). Afterloading of the graphite bed inside the cup, a second quartz frit (1711)is installed; this system is defined as the cup assembly. Prior toinstalling the cup assembly, the foil (1713) is used to line the insidesurface of the reactor wall. The cup assembly is then placed within thenickel reactor body (1707) and foil (1713). After the cup assembly isinstalled, a 99.9999_(wt)% pure graphite cap (1712) is screwed onto thereactor body. The cap secures the cup from movement after assembly.

PtIrGG Reactor:

Referring to FIG. 17C, the reactor body (1714) is based on a high puritygraphite rod. The graphite rod, with an outside diameter of 15.873 mm(OD) is bored through then machined on one end to have an insidediameter of 11.68 mm (ID). The inside diameter allows for theinstallation of a graphite cup (1715) for reactor wall isolation fromthe carbon bed. The carbon reaction medium is housed inside a 99.9999 wt% pure graphite cup (1715). To load the reactor, a quartz frit (1716) isplaced inside the graphite cup to form the bottom containment. 100 mg ofcarbon (1717) is then packed into the cup. After loading of the graphitebed inside the cup, a second quartz frit (1718) is installed; thissystem is defined as the cup assembly. The cup assembly is then placedwithin the graphite reactor body (1714). After the cup assembly isinstalled, a cap (1719) composed of platinum and 10% wt iridium isscrewed onto the reactor body. The cap secures the cup from movementafter assembly.

The residence time of the starting material within the reactor iseffective to instantiate product into the starting material and can bebetween 0 and 15 minutes.

Preferred reactors used in the methods of the invention are shown in thetable below.

Reactor Cup Cap Reactor Pole Chamber ID Material Material MaterialMaterial Boundary Capacity Coil Type CgF N/A N/A Cu, Ni or graphite N/A100 mg Induction Mo or graphite CuG Graphite graphite Cu quartz N/A 100mg Induction or Frequency PtIrGG Graphite Pt/Ir graphite quartz N/A 100mg Induction GPtG Graphite graphite graphite quartz Pt 100 mg Inductionor Frequency GPtGPtG Graphite graphite graphite quartz 2X Pt 100 mgInduction GG-EL Graphite graphite graphite quartz N/A 100 mg-3 gInduction or Frequency Foil (Pt) Graphite graphite graphite quartz Pt100 mg Induction or Frequency GZ Foil Graphite graphite graphite quartzNb, Co 100 mg Induction or or any Frequency nZG Foil Graphite Any Zgraphite quartz Ir 100 mg Induction or Frequency NiG Graphite graphiteNi quartz N/A 100 mg Induction or Frequency NiPtG Graphite graphite Niquartz Pt 100 mg Induction ZG N/A Pd/Ru or graphite quartz N/A 100 mgInduction any Z Ref-X Graphite graphite graphite quartz N/A 1-20 gFrequency.

The invention further relates to methods of instantiating elementalmetals in nanoporous carbon powders to produce nanoporous carboncompositions. Instantiating is defined herein to include the nucleation,assembly and agglomeration of metal atoms within carbon structures,particularly, ultramicropores. Without being bound by theory, it isbelieved instantiation is related to, inter alia, degrees of freedom ofthe electromagnetic field as expressed by quantum field theory. Byexposing a gas to harmonic resonances, or harmonics, of electromagneticradiation within one or more ultramicropores, vacuum energy density isaccessed and allows for the nucleation and assembly of atoms.Electromagnetic energy that is within the frequencies of light, x-rays,and magnetic fields subjected to frequency generators can enhance theformation and maintenance of such harmonics. Modifying the boundaries ofthe system, by selecting the reactor materials and adding a foil layercan also enhance the harmonics.

In particular, the invention includes processes of producing, orinstantiating, nanoporous carbon compositions comprising the steps of:

adding a nanoporous carbon powder into a reactor assembly as describedherein;

adding a gas to the reactor assembly;

powering the one or more RA coils to a first electromagnetic energylevel;

heating the nanoporous carbon powder;

harmonic patterning the nanoporous carbon powder between a firstelectromagnetic energy level and a second electromagnetic energy levelfor a time sufficient to instantiate an elemental metal nanostructure ina nanopore.

The term “harmonic patterning” is defined herein as oscillating betweentwo or more energy levels (or states) a plurality of times. The energystates can be characterized as a first, or high, energy level and asecond, or lower, energy level. The rates of initiating the first energylevel, obtaining the second energy level and re-establishing the firstenergy level can be the same or different. Each rate can be defined interms of time, such as over 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 or moreseconds. Each energy level can be held for a period of time, such as 1,2, 3, 4, 5, 6, 7, 8, 9, 10 or more seconds. Harmonic patterning iscontinued until instantiation is achieved.

Where two more electromagnetic radiation sources are present (e.g.,coils, x-ray source, lasers, and/or lamps), each can be subjected toharmonic patterning and the patterning can occur independently,simultaneously or sequentially.

The process further comprises independently powering any additionalelectromagnetic radiation source, as described above in the E/MEEapparatus or reactor assembly. For example, the process furthercomprises the step(s) of powering RA frequency generator(s) connected toone or more RA coils, one or more lamps or lasers, x-ray sources,induction coils, E/MEE coils, and the like substantially as describedabove.

The invention further includes processes of quantum printing metal atomson nanoporous carbon compositions comprising the steps of:

adding a nanoporous carbon powder into a reactor assembly as describedherein;

adding a gas to the reactor assembly;

powering the one or more RA coils to a first electromagnetic energylevel;

heating the nanoporous carbon powder;

harmonically patterning the nanoporous carbon powder between a firstelectromagnetic energy level and a second electromagnetic energy levelfor a time sufficient to instantiate an elemental metal nanostructure ina nanopore.

Ex. 1: Energy/Light Combed Activation (E/LC)

One hundred milligrams (100 mg) of powdered carbon was placed in agraphite tubular reactor (15.875 mm) OD, with ID machined to ˜9 mm), asdescribed above. Research-grade helium (He) was delivered at 2 SLPM topurge the system for a minimum of 25 seconds or more. The gases were fedthrough the E/MEE in a horizontal and level gas line, as describedabove.

Referring to FIG. 1, the argon “KC” light 108 located in position 0(vertical lamp orientation; 7.62 cm from inlet or entrance flange; at180°; bulb tip pointing up 2.54 cm from the outer diameter of the gasline) was turned on at the onset while simultaneously energizing thepower supply to 5 amps. This light was kept on for a minimum hold timeof 9 sec. Next light 109 in position 1 (109; horizontal lamporientation; 7.62 cm from inlet or entrance flange; at 180°; bulb tipfacing exit plate; bulb glass base at the optical entrance; 5.08 cm,from the outer diameter of the gas line), a krypton light, was turned onand the power is increased to 10 amps on the power supply. This was heldfor 3 seconds, light 107, in position 1 (107; horizontal lamporientation; at 0°; bulb tip at the optical exit facing the exit plate;5.04 cm from the outer diameter of the gas line), a xenon light wasturned on and held for 9 seconds and the power was increased to 15 amps.After these 3 lights have been sequentially turned on, the amperagedelivered to reactor was adjusted to 54 amps and held for a minimum of40 seconds. Immediately after the power was increased light 103 inposition 1 (103; vertical lamp orientation; 7.62 cm from inlet orentrance flange; at 0°; bulb tip pointing down 2.54 cm from the outerdiameter of the gas line), a neon light, was turned on.

Amperage “harmonic patterning” was then initiated on the reactor. Witheach amperage pattern (oscillation), the gases fed to the reactor cantreated by the same or different light sequence. In one embodiment ofthe experimental protocol, the amperage of the reactor was increased to74 amps over 1 second, the high end harmonic pattern point. The amperageof the reactor was then decreased to 34 amps over 9 seconds and held at34 amps for 3 seconds. Immediately at the start of the 3 second hold, anargon light 122 in position 1 (122; horizontal lamp orientation; at180°; bulb tip pointing towards entrance plate at the optical entrance;5.04 cm from the outer diameter of the gas line) was turned on. Afterthe 3 second hold, amperage to the reactor was then ramped up to 74 ampsover 9 seconds with a 3 second hold upon reaching 74 amps before adownward ramp was initiated. The reactor amperage was decreased to 34amps, over 9 seconds and then held for 3 seconds. Immediately at thestart of the 3 second hold, light 103 (103), a neon light in position 1,was turned on. The reactor amperage was again ramped up to 74 amps over9 seconds, held there for 3 seconds, and then again ramped down to 34amps over 9 seconds. A long-wave ultraviolet lamp (104; horizontal lamporientation; at 90°; bulb tip facing entrance plate at the opticalentrance; 5.04 cm from the outer diameter of the gas line) in position 1was turned on. The reactor was again ramped up to 74 amps over 9seconds, held for 3 seconds, then decreased to 34 amps over another 9seconds. Next a short-wave ultraviolet lamp (105 horizontal lamporientation; 7.62 cm from inlet or entrance flange; at 270°; bulb tip atthe optical entrance and facing the entrance plate; 5.04 cm from theouter diameter of the gas line) in the E/MEE (position 1) E/MEE sectionlight was turned on and held for 3 seconds. The reactor was again rampedup to 74 amps over 9 seconds; during the 3 second hold, E/MEE sectionlight (106; vertical lamp orientation; centered between optical ends(FIG. 1 entrance 101, exit 110); at 0°; bulb tip pointing down 5.04 cmfrom the outer diameter of the gas line), a neon light was rotated 90°to position 2 (106; horizontal lamp orientation; at 0°; bulb tip facingexit plate; 5.04 cm from the outer diameter of the gas line). This newposition was held for 3 seconds before the reactor amperage wasdecreased to 34 amps over another 9 seconds. The reactor was then heldat 34 amps for 3 seconds, before another ramp up to 74 amps over 9seconds was initiated. At 3 seconds into this ramp, lamp 107, inposition 1 (107) was rotated 90° to position 2 and (vertical lamporientation; at 0°; bulb tip pointing up; bulb base 5.04 cm from theouter diameter of the gas line) was turned on and held there for theremaining 6 seconds of the 9 second total ramp. The reactor was held for3 seconds in this condition.

The lights were turned off simultaneously in the E/MEE section asfollows: (103), (108), (106), (105) and (104) and the reactor wasdeenergized. The reactor was held at this state, with continuous gasflow for 27 seconds. Then all remaining lights were turned off. Gascontinued to flow for 240 seconds. The sample was removed from thereactor.

Ex. 2 Gradient Sequenced Activation (GSA)

One hundred milligrams (100 mg) of nanoporous carbon powder was placedin a graphite tubular reactor (15.875 mm OD, with ID machined to ˜9 mm)as illustrated in FIG. 2A. The powder was contained within the innerreactor using two porous frits which allow gas flow into and out of thereactor while trapping the powder. A fixed (packed) bed was used with astandard or reverse field coil. This reactor assembly was then placedwithin a quartz outer-containment vessel, which provides both gascontrol and a sealed system. Gases were delivered to the reaction zonefrom pressurized gas cylinders controlled by mass flow meters (Porterthermal mass flow meters). A Pall Gaskleen AT Purifier was installedimmediately after the CO gas cylinder for carbonyl filtration atflowrates up to 5 SLPM and particulate filtration to 0.003 μm.

Research grade N₂ is introduced into the system as reaction gas andcarrier of electromagnetic information embedded in its concentrationgradient. The gas is introduced at a constant flowrate of 2 SLPM intothe reactor until a concentration of at least 99.5% vol is reached atthe reactor assembly inlet an entrance boundary condition for theoscillating magnetic field (to maintain the concentration profile forstabilizing information). Reaction/information carrier gas either passedthrough the E/MEE (as described above in Ex. 1) or bypassed the E/MEEthrough non-transparent Tygon tubing 6.25 mm OD with an approximatelength of 2.4 m (8 feet), allowing for a residence time of 8 secondsbetween the gas manifold and the reactor inlet. The information carriergas was maintained for a minimum of 25 seconds. At the completion of thegas induction period, the reactor power supplied to the induction coiloperated at variable frequencies with a standard oscillating magneticfield (nominally 222 kHz). The induction coil was powered at 100 ampsfor a minimum of 35 seconds to satisfy information embeddingrequirements. The power is then reduced to 58.5 amps, providing a newset of oscillating field parameters to satisfy network informationembedding requirements. At this time the carrier gas was secured toinduce a reverse gradient created via application of inverse pressurevia a vacuum condition. The vacuum was maintained for ˜240 seconds tostabilize and fortify the embedded information network. The reactorpower was then secured, and the reactor was allowed to cool for ˜240seconds. The reactor was then opened to atmospheric conditions andsamples recovered for analysis.

In the baseline experiment, the nanoporous carbon powder was a 200 meshgraphite (Alfa Aesar, >99.9995% wt pure).

Ex. 3: Reduced Gradient Activation (GSR)

One hundred milligrams (100 mg) of nanoporous carbon powder was placedin a graphite tubular reactor (15.875 mm OD, with ID machined to ˜9 mm)as illustrated in FIG. 2A. Research grade N₂ is introduced into thesystem as reaction gas and carrier of electromagnetic informationembedded in its concentration gradient. The gas is introduced at aconstant flowrate of 2 SLPM into the reactor until a concentration of atleast 99.5% vol is reached at the reactor assembly inlet an entranceboundary condition for the oscillating magnetic field (to maintain theconcentration profile for stabilizing information). Reaction/informationcarrier gas either passed through the E/MEE (as described above inEx. 1) or bypassed the E/MEE through non-transparent Tygon tubing 6.35mm OD with an approximate length of 2.4 m (8 feet), allowing for aresidence time of 8 seconds between the gas manifold and the reactorinlet. The information carrier gas was maintained for a minimum of 25seconds. At the completion of the gas induction period, the reactorpower supplied to the induction coil operated at variable frequencieswith a standard oscillating magnetic field (nominally 222 kHz). Theinduction coil was powered at 40 amps for a minimum of 35 seconds toinduce information network formation. The power is then reduced to 25amps, providing a new set of oscillating field parameters to stabilizethe embedded information network. At this time the carrier gas wassecured to induce a reverse gradient created via application of inversepressure via a vacuum condition. The vacuum was maintained for ˜240seconds to stabilize and fortify the embedded information network. Thereactor power was then secured, and the reactor was allowed to cool for˜240 seconds. The reactor was then opened to atmospheric conditions andsamples recovered for analysis.

In the baseline experiment, the nanoporous carbon powder was a 200 meshgraphite (>0.74 mm) (Alfa Aesar, >99.9995%_(wt) pure).

Ex. 4: Site Activation Harmonic Resonance (Mini-X)

One hundred milligrams (100 mg) of powdered carbon was placed in agraphite tubular reactor (15.873 mm OD, with ID machined to ˜9 mm), asillustrated in FIG. 2C. Research-grade helium (He) was delivered at 2SLPM to purge the system for a minimum of 25 seconds or more. The gaseswere fed through the E/MEE (as described above in Ex. 1). In thisexample, a fixed (packed) bed was used with three coils and a mini-Xx-ray tube. This reactor assembly was then placed within a quartzouter-containment vessel, which provides both gas control and a sealedsystem. Gases were delivered to the reaction zone as described above.

Research-grade Helium (He) was delivered at 2 SLPM to the reactorassembly, bypassing the E/MEE section, through non-transparent Tygontubing 6.35 mm OD with an approximate length of ˜2.5 m, allowing for aresidence time of 8 seconds between the gas manifold and the reactorsystem inlet. This gas purge was maintained for a minimum of 25 seconds(or longer) to allow at least three system turnovers (>3× volume purge).At the completion of the purge period, the Mini-x (211) power was turnedon and held for 2 seconds. After the 2 second hold, a 405 nm Laser (212)directed through the reactor bed was turned on, immediately followed byfrequency generator 2 controlling the second of three coils and thenfrequency generator 1 controlling the first of three coils. Initially,frequency generator 2 creates harmonic patterns from 626 Hz to 2.83 MHzsine wave ramping at a rate of 3 seconds up and 3 seconds downs for 1complete harmonic pattern followed by 157 Hz to 557 KHz sine wave with a6 second ramp up and down with 2 complete cycles followed by 157 Hz to557 kHz sine wave with a 9 second ramp up and down with 6 completecycles. Initially, frequency generator 1 creates harmonic patterns from987 Hz to 2.83 MHz triangle wave ramping at a rate of 3 seconds up and 3seconds downs for 1 complete harmonic pattern followed by 10 Hz to 987Hz triangle wave with a 6 second ramp up and down with 2 complete cyclesfollowed by 10 Hz to 987 Hz triangle wave with a 9 second ramp up anddown with 6 complete cycles. After the first harmonic pattern cycle forboth frequency generators were completed, gas was secured, discontinuingall new flow into the system, and a vacuum system was initiated to pullthe gases. This vacuum was held for ˜151 seconds or longer, allowingequilibration of the powder within the reactor system. Immediately afterthe vacuum condition was started, frequency generator 3 was turned on.Initially, frequency generator 3 controlling the third coil createdharmonic patterns from 257 kHz to 263 kHz square wave ramping at a rateof 3 seconds up and 3 seconds downs for 4 complete harmonic patternfollowed by 257 kHz to 263 kHz square wave with a 6 second ramp up anddown with 6 complete cycles followed by 257 kHz to 263 kHz square wavewith a 9 second ramp up and down and 3 complete cycles. At 150 secondsplus 600 milliseconds of the vacuum hold, frequency generators 1 and 2were secured. At 150 seconds plus 809 milliseconds, frequency generator3 was secured. At the end of the 151 second vacuum condition, anadditional 3 second hold without the presence of vacuum was initiated.Following the 3 second hold both the 405 nm laser (212) and mini-X (211)were secured. The sample was removed.

Ex. 5: Site Activation Harmonic Resonance (Active)

One hundred milligrams (100 mg) of powdered carbon was placed in agraphite tubular reactor (15.875 cm OD, with ID machined to ˜9 mm) withthree wire windings (or coils) each connected to a power source andfrequency generator, as shown in FIG. 2C. The powder was containedwithin the inner reactor using two porous frits designed to allow gasflow into and out of the reactor while trapping the powder. This reactorassembly was then placed within a sealed quartz outer-containment vesselas described above.

Research-grade Helium (He) was delivered at 2 SLPM to the reactorassembly. The gases bypass the E/MEE section, passing throughnon-transparent Tygon tubing 6.35 mm OD with an approximate length of˜2.5 m, allowing for a residence time of 8 seconds between the gasmanifold and the reactor system inlet. This gas purge was maintained fora minimum of 25 seconds (or longer) to allow at least three systemturnovers (>3× volume purge). At the completion of the purge period, thefirst and second frequency generators (1 and 2) connected to two coilswere turned on and the frequency harmonic patterning started. Initiallyfrequency generator 2 generated harmonic patterns from 626 Hz to 2.83MHz sine wave ramping at a rate of 3 seconds up and 3 seconds downs for1 complete harmonic pattern followed by 157 Hz to 557 kHz sine wave witha 6 second ramp up and down with 2 complete cycles followed by 157 Hz to557 kHz sine wave with a 9 second ramp up and down with 6 completecycles. Initially frequency generator 1 generated harmonic pattern from987 Hz to 2.83 MHz triangle wave ramping at a rate of 3 seconds up and 3seconds downs for 1 complete harmonic pattern followed by 10 Hz to 987Hz triangle wave with a 6 second ramp up and down with 2 complete cyclesfollowed by 10 Hz to 987 Hz triangle wave with a 9 second ramp up anddown with 6 complete cycles. After the first harmonic pattern cycle forboth frequency generator 1 and 2 were completed, gas was secured,discontinuing all new flow into the system, and a vacuum was initiated.The vacuum was held for ˜152 seconds or longer. Immediately after thevacuum condition was started, frequency generator 3 connected to thethird coil was turned on and the frequency harmonics started. Initiallyfrequency generator 3 generated harmonic patterns from 257 kHz to 263kHz square wave ramping at a rate of 3 seconds up and 3 seconds downsfor 4 complete harmonic patterns followed by 257 kHz to 263 kHz squarewave with a 6 second ramp up and down with 6 complete cycles followed by257 kHz to 263 kHz square wave with a 9 second ramp up and down and 3complete cycles. At 133 seconds plus 200 milliseconds of the vacuumhold, frequency generators 1 and 2 were secured. At 151 seconds plus 600milliseconds, frequency generator 3 was secured. At the end of the 152second vacuum condition, an additional 15 second hold without thepresence of vacuum was initiated. The sample was removed.

Ex. 6: Site Activation Harmonic Resonance (Static)

One hundred milligrams (100 mg) of powdered carbon was placed in agraphite tubular reactor (15.875 mm OD, with ID machined to ˜9 mm) withthree wire windings or coils, as shown in FIG. 2C.

Research-grade nitrogen gas was delivered at 2 SLPM to the reactorassembly. The gas bypassed the E/MEE section, as described above. A gaspurge was maintained for a minimum of 25 seconds (or longer). At thecompletion of the purge period, frequency generator 2 and then frequencygenerator 1, connected to two coils, were turned on. Frequency generator2 generated harmonic patterns from 626 Hz to 2.83 MHz sine wave rampingat a rate of 3 seconds up and 3 seconds downs for 6 complete harmonicpatterns followed by 157 Hz to 557 kHz sine wave with a 9 second ramp upand down with 3 complete cycles followed by 157 Hz to 557 kHz sine wavewith a 6 second ramp up and down with 10 complete cycles. Frequencygenerator 1 generated harmonic patterns from 987 Hz to 2.83 Mhz trianglewave ramping at a rate of 3 seconds up and 3 seconds downs for 6complete harmonic pattern followed by 10 Hz to 987 hz triangle wave witha 9 second ramp up and down with 2 complete cycles followed by 10 Hz to987 hz triangle wave with a 6 second ramp up and down with 10 completecycles. After the first harmonic pattern cycle for both frequencygenerator 1 and 2 was completed, gas was secured, discontinuing all newflow into the system, and a vacuum system was initiated to pull thegases. The vacuum was held for ˜183 seconds or longer. Immediately afterthe vacuum was started, frequency generator 3 was turned on and thefrequency harmonic patterns started. Frequency generator 3 was broughtto 1.7 MHz square wave. At 174 seconds of the vacuum hold, frequencygenerators 1 and 2 were secured. After an additional 182.6 seconds,frequency generator 3 was secured. The vacuum was discontinued for anadditional 15 seconds. The sample was removed.

Ex. 7: Ref-X Conditioning—Static Pre-Conditioning

One gram (1 g) of powdered carbon was placed in a graphite tubularreactor (44.5 mm OD, with ID machined to ˜25 mm) as shown in FIG. 4B.The gases pass through an E/MEE section, as generally described inEx. 1. Research-grade nitrogen was delivered at 2 SLPM to the reactorassembly. A purge was maintained for 90 seconds. The reactor assemblywas then installed in a Desorb conditioning oven, preheated to 176 C(350° F.). After 30 seconds, frequency generator 1 was turned on.Frequency generator 1 generated harmonic patterns from 0.001 Hz to 3.5MHz sine wave ramping at a rate of 9 seconds up and 9 seconds downs for33 complete harmonic patterns followed by 0.001 Hz to 3.5 MHz trianglewave ramping at a rate of 9 seconds up and 9 seconds downs for 34complete harmonic patterns followed by 0.001 Hz to 3.5 MHz square waveramping at a rate of 9 seconds up and 9 seconds downs for 33 completeharmonic patterns followed by 827 Hz to 2.83 MHz sine wave ramping at arate of 6 seconds up and 6 seconds downs for 30 complete harmonicpatterns followed by 827 Hz to 2.83 MHz triangle wave ramping at a rateof 7 seconds up and 5 seconds downs for 30 complete harmonic patternsfollowed by 827 Hz to 2.83 MHz square wave ramping at a rate of 7seconds up and 5 seconds downs for 40 complete harmonic patternsfollowed by 827 Hz to 2.83 MHz square wave ramping at a rate of 5seconds up and 7 seconds downs for 50 complete harmonic patternsfollowed by 235.5 kHz to 474 kHz triangle wave ramping at a rate of 2seconds up and 4 seconds downs for 100 complete harmonic patternsfollowed by 235.5 kHz to 474 kHz sine wave ramping at a rate of 2seconds up and 4 seconds downs for 100 complete harmonic patterns thenby 235.5 kHz to 474 kHz square wave ramping at a rate of 2 seconds upand 4 seconds downs for 100 complete harmonic patterns. Thirty secondsafter the initiation of the frequency harmonic patterns, 403 light wasturned on in E/MEE (FIG. 4A). After a 60 second hold, 402 was turned onand held for 1745 seconds. 404 was then turned on and held for 360seconds. 403 was then rotated 90° to position 2 and held for 6 seconds.402 was then rotated 90° to position 2 and held for 4 seconds. 408 wasthen turned on and held for 395 seconds. 408 was then rotated 90° toposition 2 and held for 35 seconds. 405 was then turned on and held for347 seconds. 406 was then turned on and held for 6 seconds. 408 was thenrotated 90° back to position land held for 5 seconds. 405 was thenturned off and held for an additional 600 seconds. The frequencygenerators were paused while the reactor assembly was removed from theoven and placed on a heat resistant platform while maintaining gas flow.The frequency harmonic patterns were immediately restarted. 406 wasrotated to position 2 and held for 36 seconds. 406 was then rotated toposition 1 and held for 126 seconds. 408 was then rotated to position 2and held for 600 seconds. 408 was then rotated to position 1 and heldfor 840 seconds. 408 was then rotated to position 2 and held for 184seconds. 408 was then rotated to position 1 and held for 6 seconds. 403was then rotated to position 1, turned off and held for 9 seconds.Frequency generator 1 was secured; 408 & 406 were turned off and heldfor 9 seconds. 404* and then 402 were turned off and held for 90seconds. Gas flow was secured and the reactor assembly was disconnectedfrom the gas feed line. The carbon bed was removed.

Ex. 8: Ref-X Conditioning—Static

One gram (1 g) of powdered carbon was placed in a graphite tubularreactor (44.45 mm OD, with ID machined to ˜25 mm), as shown in FIG. 4B.A fixed (packed) bed is used with three wire windings or coils.

Research-grade Neon (Ne) gas was delivered at 2 SLPM to the reactorassembly. The gas passed through the E/MEE section. A gas purge wasmaintained for a minimum of 90 seconds (or longer) to allow at leastthree system turnovers (>3× volume purge). At the completion of thepurge period, the 404 was turned on immediately followed by 402 and heldfor 8 seconds. The coil in the E/MEE was energized and using frequencygenerator 4. Frequency generator 4 provided a constant 1.697 MHz Squarewave signal to the coil (407). Immediately after Frequency generator 4is started, 408 was turned on immediately followed by the turning on theMini-X x-ray source (424) followed by a 2 second hold. A 405 nm laser(427) was turned on immediately followed by a 532 nm laser (426) andheld for 22 seconds. The following lights were powered in the followingsequence: 415 & 418, 416 & 419, 417 & 420, and 406 which were then heldfor 9 seconds. 402 was then rotated 90° to position 2 immediatelyfollowed by a change in the incoming gas from Neon (Ne) to Nitrogen (N2)and held for 90 seconds. 406 was then rotated 90° to position 2 and heldfor 3 seconds. 415 was turned off and 4034 was immediately rotated 90°to position 2 and held for 6 seconds. 415 was turned on and held for 3seconds. 406 was then rotated 90° to position 1 and held for 4 seconds.404 was turned off and held for 2 seconds. 406 was turned off and heldfor 27 seconds. The frequency generator 2 and then frequency generator 1were turned on and held for 5 second hold. Initially frequency generator2 generated harmonic patterns from 626 Hz to 2.83 MHz sine wave rampingat a rate of 3 seconds up and 3 seconds downs for 20 complete harmonicpatterns followed by 157 Hz to 557 Khz sine wave with a 9 second ramp upand down with 8 complete cycles followed by 157 Hz to 557 Khz sine wavewith a 6 second ramp up and down with 10 complete cycles. Initiallyfrequency generator 1 generated harmonic patterns from 987 Hz to 2.83MHz triangle wave ramping at a rate of 3 seconds up and 3 seconds downsfor 20 complete harmonic pattern followed by 10 Hz to 987 Hz trianglewave with a 9 second ramp up and down with 8 complete cycles followed by10 Hz to 987 Hz triangle wave with a 6 second ramp up and down with 10complete cycles. Five seconds after the frequency generators began, 418and 416 were turned off and held for 1 second. 418 and lower 416 werethen turned on. 419 and 420 were then turned off and held for 1 second.419 and 420 were then turned on and held for 27 seconds. Frequencygenerator 4 was shut down and 408 was turned off, immediately followedby turning off 402 and held for 87 seconds. Incoming gas flow wassecured, and a vacuum was started and held for 18 seconds. 403 wasturned off and held for 72 seconds. 405 was turned on and frequencygenerator 3 was started at a fixed frequency of 1.697 MHz square waveand held for 54 seconds. Both frequency generators 1 and 2 were securedand held for 123 seconds. Frequency generator 3 and the vacuum systemwere secured and held for 3 seconds. 415, 416, 417, 418, 419, and 420are turned off simultaneously and held for 3 seconds. 424 and 427 werethen shut off simultaneously. The 426 was then shut off and held for 3seconds. 404 was turned off and held for 15 seconds. The samples werethen removed.

Ex. 9: Ref-X Conditioning—Eversion

One gram (1 g) of powdered carbon is placed in a graphite tubularreactor (44.45 mm OD, with ID machined to ˜25 mm), as shown in FIG. 4B.

Research-grade Neon (Ne) gas was delivered at 2 SLPM to the reactorassembly. During the purge, gases passed through the E/MEE section. Thisgas purge was maintained for a minimum of 90 seconds to allow at leastthree system turnovers (>3× volume purge). At the completion of thepurge period, the 404 was turned on immediately followed by 402 then an8 second hold was started. At the end of the 8 second hold, the coil(407) in the E/MEE was energized. Frequency generator 4 started harmonicpatterns from 557 Hz to 157 kHz sine wave ramping at 9 seconds up and 3seconds down to the coil until shutdown. Immediately after Frequencygenerator 4 was started, 408 was turned on immediately followed by theturning on of the Mini-X x-ray source (427) followed by a 2 second hold.A 405 nm laser was then turned on immediately followed by a 532 nm laser(426) followed by a 22 second hold period. The following lights werethen turned on in the following sequence, 415 & 418, 416 & 419, 417 &420, then 406 followed by a 9 second hold. 402 was then rotated 90° toposition 2 immediately followed by a change in the incoming gas fromNeon (Ne) to Nitrogen (N2) followed by a 90 second hold. 406 was thenrotated 90° to position 2 followed by a 3 second hold. 415 was thenturned off immediately followed by 403 rotated 90° to position 2followed by a 6 second hold. 415 was then turned on followed by a 3second hold. 406 was then rotated 90° to position 1 followed by a 4second hold. 404 was then turned off followed by a 2 second hold. 406was then turned off followed by a 27 second hold. Frequency generator 2and then frequency generator 1 were then turned on and their frequencyharmonic patterns started followed by a 5 second hold. Frequencygenerator 2 started harmonic patterns from 626 Hz to 2.83 MHz sine waveramping at a rate of 3 seconds up and 3 seconds downs for 20 completeharmonic patterns followed by 157 Hz to 557 kHz sine wave with a 9second ramp up and down with 8 complete cycles followed by 287.5 kHzsine wave and held until termination. Frequency generator 1 startedharmonic patterns from 987 Hz to 2.83 MHz triangle wave ramping at arate of 3 seconds up and 3 seconds downs for 20 complete harmonicpattern followed by 10 Hz to 987 Hz triangle wave with a 9 second rampup and down with 8 complete cycles followed by 285 Hz triangle wave andheld until termination. After the 5 second hold, 418 and 416 were turnedoff and held for 1 second. 418 and 416 were then turned on. 419 and 420were then turned off and held for 1 second. 419 and 420 were turned onand held for 27 seconds. Frequency generator 4 was shut down and 408 wasturned off. 402 was immediately turned off and held for 87 seconds.Incoming flow was secured, and a vacuum was started on the system andheld for 18 seconds. 403 was turned off and held for 72 seconds. 405 wasturned on. Frequency generator 3 was started and the frequency was setat a fixed frequency of 1.697 MHz square wave for 240 seconds followedby 28.25 MHz to 28.75 MHz square wave cycling at 3 seconds up and downfor 22 cycles and then 1.697 MHz square wave signal until termination.At the end of the 174 seconds of the 240 second hold on frequencygenerator 3, both frequency generator 1 and 2 were secured and a 1second hold started. At the end of the 1 second hold, frequencygenerator 3 and the vacuum system were secured and a 3 second holdstarted. At the end of the 3 second, the following lights, 415, 416,417, 418, 419, and 420 were turned off simultaneously, followed by a 3second hold. The 424 and 427 were then shut off simultaneously. The 426was then shut off and a 3 second hold was started. At the end of the 3second hold time, 404 was turned off and a 15 second hold was started.At the end of the 15 second hold, the sample was removed.

Below is a table of the experiments performed with positive results:

Illus- Carbon Other Carbon Reactor tration Protocol Form Pretreatment IDGas 1 GSA Graphite Z ZG N2 2 GSA Graphite Z CuG N2 3 GSA Graphite ZGPtGPtG He 4 GSA Graphite Z NiPtG N2 5 GSA Graphite Z NiPtG He (at 750C)6 GSA Graphite Z PtIrGG He 7 GSA Graphite R CuG N2 8 Mini-X Graphite RGG-EL N2 9 E/LC APKI CgF Kr 10 GSA APKI CuG N2 11 GSA APKI 350C DesorbCuG N2 12 E/LC PEEK GG-EL CO 13 GSA PEEK CuG N2 14 GSA MSP20X CuG N2(raw) 15 GSR Lot 2006 24% CO2 GG-EL N2 350C Desorb 16 GSA Lot 2006 12%RH GG-EL N2 Soak 17 GSA Lot 1000 CuG N2 18 GSA Lot 1002 CuG N2 19 GSALot 1013 GG-EL N2 20 GSA MSC30 GPtG He (raw) 21 GSR Lot 2008 GG-EL N2 22GSA Lot 2003 CuG N2 23 GSA Lot 2003 125C Desorb CuG N2 24 GSA Lot 2003250C Desorb CuG N2 25 GSA Lot 2003 350C Desorb CuG N2 26 E/LC GSX (raw)GG-EL/ He GZ(Co) 27 E/LC Lot 2005 40% RH GG-EL He Soak 28 GSA Lot 200570% RH GG-EL N2 soak 29 GSR Lot 2005 12% RH GG-EL N2 Soak 30 GSR Lot2005 GG-EL/ He GZ-(Pt) 31 E/LC Graphite Z GZ (Nb) He 32 E/LC Graphite ZGZ(Co) He 33 E/LC Graphite Z NiG N2 34 GSA Graphite Z ZG (Z = N2 Cu/Rx =G) 35 GSA Graphite Z ZG (Rx = N2 Cu/Z^(ins) = G) 36 E/LC MSC30 NiG He(raw) 37 E/LC Graphite Z CgF Mix 2 38 E/LC Graphite A Lollipop Mix 1 39QPP-PFC Lot 1044 GG-EL N2 (static) 40 QPP-PFC 20% Lot 350C Desorb GG-ELN2 (static) 1044 80% Lot 1045 41 QPP-PFC Lot 2006 70% GG-EL He (static)RH Soak 24% CO2 42 QPP-PFC MSP20X CuG N2 (active) (raw) 43 QPP-PCC Lot2000 CuG He/H2 (active 44 QPP-PFC MSP20X CuG N2 (active) (raw) 45 Ref-XRef-X Ref-X Mix 3 Static Blend 46 Ref-X Ref-X Ref-X Mix 3 Static Blend47 Ref-X Ref-X Ref-X Mix 3 Static Blend 48 Ref-X Ref-X Ref-X Mix 3Eversion Blend 49 Ref-X Ref-X Ref-X Mix 3 Eversion Blend 50 QPP-PFCMSP20X CuG He/H2 (static) (raw) Mix 1 = CO(50%):Kr(35%):He(15%) Mix 3 =Ne followed by N2

Elements were detected in accordance with the above illustrations areset forth in the periodic table found in FIG. 16A-16E. Startingmaterials resulted in instantiation in accordance with the followingtable.

Starting Material Si Ca Ti V Cr Mn Fe Co Ni Cu Zn Y Zr Nb Mo Ce W PbC_(graphite) 12 2 7 9 3 5 112 20 11 8 6 C_(nano) 53 19 7 3 36 4 3 16 513 1 23 7 3 8 4 19 C_(act) N/R 1 6 1 38 3 1 1 1 6 32 1 3 C_(MCG)  6 3 3 22 1 3 1 6 .

The patent and scientific literature referred to herein establishes theknowledge that is available to those with skill in the art. All UnitedStates patents and published or unpublished United States patentapplications cited herein are incorporated by reference. All publishedforeign patents and patent applications cited herein are herebyincorporated by reference. All other published references, documents,manuscripts and scientific literature cited herein are herebyincorporated by reference.

While this invention has been particularly shown and described withreferences to preferred embodiments thereof, it will be understood bythose skilled in the art that various changes in form and details may bemade therein without departing from the scope of the inventionencompassed by the appended claims. Numerical values where presented inthe specification and claims are understood to be approximate values(e.g., approximately or about) as would be determined by the person ofordinary skill in the art in the context of the value. For example, astated value can be understood to mean within 10% of the stated value,unless the person of ordinary skill in the art would understandotherwise, such as a value that must be an integer.

What is claimed is:
 1. A reactor assembly comprising: a gas inlet andone or more gas outlets; a reactor chamber containing a nanoporouscarbon material disposed within a cup and covered with a cap; a firstporous frit defining a floor of the reactor chamber disposed within thecup, a second porous frit defining the ceiling of the reactor chamberand disposed below the cap; wherein each porous frit has a porosity thatis sufficient to allow a gas to permeate into the reactor chamber andcontain a nanoporous carbon material; a reactor head space disposedabove the reactor cap; an foil disposed between the reactor chamber andreactor cup; an x-ray source configured to expose the reactor head spaceto x-rays; one or more lasers configured to direct a laser towards afrit and/or through the reactor chamber 2, 3, 4, 5 or more RA coils eachRA coil independently comprising a wire winding surrounding the reactorchamber and/or reactor head space operably connected to one or more RAfrequency generators and one or more power supplies; 2, 3, 4, 5 or morepairs of RA lamps wherein the pairs of RA lamps are disposedcircumferentially around the RA coils and define a space between thepairs of RA lamps and the RA coils; and a computer processing unitconfigured to control the power supply, and frequency generator.
 2. Thereactor assembly of claim 1, wherein the cup is composed of graphite. 3.The reactor assembly of claim 1, wherein the cap is composed ofgraphite, platinum, palladium or ruthenium.
 4. The reactor assembly ofclaim 1, wherein the foil envelops the cup.
 5. The reactor assembly ofclaim 4, wherein the foil is composed of platinum.
 6. The reactorassembly of claim 1, further comprising a pole disposed below thereactor chamber and above the gas inlet.
 7. The reactor assembly ofclaim 6, wherein the pole is composed of quartz.
 8. The reactor assemblyof claim 1, wherein the reactor chamber is sized to hold about 100 mgnanoporous carbon material.
 9. The reactor assembly of claim 1, wherein:the gas inlet is in fluid connection with at least one gas supplyselected from the group consisting of air, oxygen, hydrogen, helium,nitrogen, neon, argon, krypton, xenon, carbon monoxide, carbon dioxideand mixtures thereof; the gas supplies are free of metal salts andvaporized metals; and the gas supply is directed through a gas manifoldcontrolled by mass flow meters.
 10. The reactor assembly of claim 1,wherein the nanoporous carbon powder comprises graphene having at least95% wt. carbon (metals basis), a mass mean diameter between 1 μm and 5mm, and an ultramicropore surface area between about 100 and 3000 m²/g.11. The reactor assembly of claim 10, wherein the nanoporous carbonpowder is characterized by acid conditioning, wherein the acid isselected from the group consisting of HCl, HF, HBr, HI, sulfuric acid,phosphoric acid, carbonic acid, and nitric acid, and a residual watercontent of less than that achieved upon exposure to a relative humidity(RH) of less than 40% RH at room temperature.
 12. The reactor assemblyof claim 1, wherein a first RA coil comprises a copper wire winding, asecond RA coil comprises a braiding of copper wire and silver wire, anda third RA coil is a platinum wire winding and each RA coil isconfigured to create a magnetic field and wherein each power supplyindependently provides AC and/or DC current.
 13. The reactor assembly ofclaim 1, comprising 5 RA coils surrounding the reactor chamber and/orreactor head space operably connected to one or more RA frequencygenerators and one or more power supplies; wherein a first RA coil isaligned with the first frit, a second RA coil is aligned with thereactor chamber, a third RA coil is aligned with the second frit, afourth RA coil is disposed between the first RA and the second RA coiland a fifth RA coil is disposed between the second RA coil and third RAcoil.
 14. The reactor assembly of claim 1, comprising at least twolasers and wherein each laser is characterized by a differentwavelength.
 15. The reactor assembly of claim 1, wherein a first pair ofRA lamps are configured in a first plane defined by a center axis and afirst radius of the reactor chamber, a second pair of RA lamps areconfigured in a second plane defined by the center axis and a secondradius of the reactor chamber and a third pair of RA lamps areconfigured in a third plane defined by the center axis and a thirdradius of the reactor chamber.
 16. The reactor assembly of claim 1,further comprising an electromagnetic embedding apparatus locatedupstream of the gas inlet comprising: one or more gas supplies; ahousing having a housing inlet and housing outlet; an upstream gas linethat is in fluid connection with each gas supply and the housing inlet;an internal gas line in fluid connection with the housing inlet andhousing outlet; a downstream gas line in fluid connection with thehousing outlet and the gas inlet; at least one E/MEE pencil lamppositioned below the internal gas line, at least one E/MEE pencil lamppositioned above the internal gas line and at least one E/MEE pencillamp positioned to the side of the internal gas line; an optional shortwave lamp and/or a long wave lamp; and an optional E/MEE coil wrappedaround the internal gas line; wherein each E/MEE pencil lamp isindependently rotatably mounted, located along the length of theinternal gas line, and powered by the power supply; wherein the centralprocessing unit independently controls powering each E/MEE pencil lampand a rotation position of each E/MEE pencil lamp.
 17. The apparatus ofclaim 16, wherein the housing is closed and opaque, the internal gasline is transparent and external gas line in fluid connection with thehousing outlet and gas inlet is opaque.
 18. The apparatus of claim 17,wherein the internal gas line is between 50 cm and 5 meters and has adiameter between 2 mm and 25 cm.
 19. The apparatus of claim 16, wherein:at least 5 E/MEE pencil lamps are located along the internal gas line;each E/MEE pencil lamp is independently placed such that itslongitudinal axis is (i) parallel to the internal gas line, (ii)disposed radially in a vertical plane to the internal gas line, or (iii)perpendicular to the plane created along the longitudinal axis of theinternal gas line or along the vertical axis of the internal gas line;and each E/MEE pencil lamp is independently affixed to one or morepivots that permit rotation between about 0 and 360 degrees with respectto the x, y, and/or z axis wherein (i) the x-axis is defined as the axisparallel to the gas line and its vertical plane, (ii) the y-axisdefining the axis perpendicular to the gas line and parallel to itshorizontal plane, and (iii) the z-axis is defined as the axisperpendicular to the gas line and parallel to its vertical plane. 20.The apparatus of claim 16, wherein at least one E/MEE pencil lamp is aneon lamp, at least one E/MEE pencil lamp is a krypton lamp, and atleast one E/MEE pencil lamp is an argon lamp.